Dissertations / Theses: 'Solvent extraction processes'

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Haupt, Petronella. "Effective solvent extraction of coal and subsequent separation processes." Diss., Pretoria : [s.n.], 2006. http://upetd.up.ac.za/thesis/available/etd-08282007-113611.

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Thesis (M. Eng.)(Chemical Engineering)--University of Pretoria, 2006.
Accompanied by a CD-ROM containing Matlab programs. Includes bibliographical references. Available on the Internet via the World Wide Web.

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Rashid, Salman Ghanem. "Studies on copper extraction with hydroxyoxime extractants for the design of hollow fibre membrane based extraction processes." Thesis, University of South Wales, 1999. https://pure.southwales.ac.uk/en/studentthesis/studies-on-copper-extraction-with-hydroxyoxime-extractants-for-the-design-of-hollow-fibre-membrane-based-extraction-processes(7e631b77-71e2-4d6e-8c03-4636d42f9f69).html.

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This work has included a review of the most relevant aspects of measurement techniques and mathematical models proposed in the literature to assess the equilibrium and mass transfer data of metal extraction by the use of chelating agents. The limitations of these techniques and models have been highlighted. Three chelating extractants diluted in EscaidllO were used to study the extraction equilibrium of copper. The extractants are 5-nonylacetophenone oxime (LIX84®), 5- dodeylsalicylaldoxime (LIX860®) and 50/50 v/v mixture of both oximes (LIX984®). The copper concentration changes in the aqueous and the organic phases were monitored by using atomic absorption spectrophotometer. Two mathematical models (a chemical model and a semi-empirical model) have been developed in this study to predict the equilibrium data of copper sulfate/hydroxyoxime system. The chemical model was found to fit all the three equilibrium systems (CuSO4/LIX84®, LIX860®and LIX984®) equally. The semi-empirical model based on Freundlich's adsorption equation was also found to fit the three systems but with less accuracy. The mass transfer characteristics and properties of copper extraction and recovery from an aqueous solution using LIX984® were studied using dispersion-based (rising drops) and dispersion-free techniques. In the dispersion-based technique the organic phase was dispersed in form of drops at the tip of hypodermic needle while the aqueous solution was used as a continuous phase. The extraction process was carried out in four different height columns under wide range of conditions. The effects of the columns' height, the dispersed and the continuous phases concentrations on the metal rate of mass transfer were investigated. It has been found in that the metal's rate of mass transfer and system's overall mass transfer coefficient have remained constant in all four columns. A model utilising the two-film theory, some of the dimensionless groups and the experimental results has been proposed in this work to calculate the local mass transfer coefficients in the dispersed phase and the continuous phase. The overall mass transfer coefficient and the calculated local coefficients were used to account for the reaction rate constant at the interface from the sum of the individual resistances to mass transfer. A dispersion-free technique consisting of a microporous hollow fibre module was used in this study to examine the mass transfer properties of the extraction and stripping processes of copper across an immobilised interface system. The extraction and re-extraction (stripping) processes in this system were conducted under a wide range of operating conditions and produced satisfactory results. In general it has been found that counter current flow arrangement gave higher concentration driving forces which were reflected in form higher metal concentrations at the extract phase. A generalised mathematical model was developed in this study which utilised Wilson's method, the experimental data, some dimensionless groups and the two-film theory to account for local resistances and predict the system's overall mass transfer coefficient. A correlation was established first to calculate mass transfer coefficients using a form of Leveque's equation which relates the two phase's physical properties and the system's parameters. The membrane mass transfer coefficient was calculated from the structural properties of the membrane material. While the resistance at the reaction interface was calculated under set of experimental conditions. The individual coefficients were then used to predict the overall mass transfer coefficient under any set of conditions by using the aditivity approach of the individual resistances to mass transfer. However, further checks and investigations are necessary to validate this model over variety of extraction systems and membrane configurations.

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Gordon, Ross John. "Improved mass transport efficiency in copper solvent extraction." Thesis, University of Edinburgh, 2009. http://hdl.handle.net/1842/5673.

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This thesis considers methods which can be employed to increase the mass of copper transferred into and out of the organic phase during the load and strip stages of commercial solvent extraction processes. Conventional 5-alkylsalicylaldoxime reagents transfer 1 mol of divalent copper per 2 mol of ligand in a neutral complex of the type [Cu(L-H)2] via a pH-swing process. New triacidic ligands have been designed which triple the molar transport of copper to form [Cu3(L-3H)2]. Until recently copper recovery by solvent extraction has been confined to oxidic ores which are leached with sulfuric acid. New leaching technologies generate high tenor copper sulfate feed streams from sulfidic ores. The conventional 5- alkylsalicylaldoxime reagents do not work effectively in conjunction with these leach processes as they do not consume the acid which is generated on loading the oxime. To address this problem ditopic zwitterionic ligands have been designed which can transfer both metal cation and attendant anion. These new metal salt reagents are diacidic, therefore not only transfer metal salts but also increase the molar transport relative to the conventional reagents. Equilibrium-modifiers are often added to improve the mass transport efficiency of conventional solvent extraction processes. The nature of their interaction with the species in solution is poorly understood. This thesis investigates their interaction with the free ligands and copper complexes to gain an understanding of their mode of action in order to rationalise the design of future modifiers to optimise recovery efficiencies. Increased molar transport is addressed in Chapter 2. The diacidic ligand 5- methylsalicylaldehyde-pivaloylhydrazide (L2) and its dinuclear copper complex [Cu2(L2-2H)2] were synthesised and characterised to gain an understanding of their speciation in solution. X-ray structural analysis of [Cu2(L2-2H)2] confirmed that the phenolate oxygen atoms bridge the copper centres rather than the amidato oxygen atoms of the hydrazone. Variable temperature magnetic susceptibility data confirm that the copper centres are antiferromagnetically coupled as expected for the Cu-OCu angle (99.6(2)°). An understanding of the coordination geometry of the dinuclear systems lead to design of triacidic ligands. A series of 3-hydrazono- and 3- hydroxyanil- 5-alkylsalicylic acids were synthesised. The prototype ligand 5-methyl 3-octanoylhydrazonosalicylic acid (L6) was demonstrated to triple molar transport and increase mass transport by 2.5 fold. Solvent extraction results indicate that copper is sequentially loaded as pH is increased. The plateaux observed in loading curves suggest formation of stable mono-, di-, and tri-nuclear copper complexes within the pH-ranges 1.75 - 2.75, 3.25 - 4.0 and > 4.25 respectively. The triacidic ligands were also demonstrated to double the molar transport of the conventional salicylaldoximes when used in 1:1 blends by formation of a ternary complex. Chapter 3 describes the incorporation of two tertiary amine groups into diacidic salicylaldehydehydrazone ligands to form dinucleating metal salt extractants. Piperidinomethyl, piperazinomethyl and dihexylamino groups were incorporated into various positions of the ligand including 3- and/or 5- positions of the salicylaldehyde or incorporated into the hydrazone. Solvent extraction results obtained for 3,5- bis((dihexylamino)methyl)salicylaldehyde-octanoic hydrazone (L20) are consistent with transfer of 1 mol of copper sulfate per mol of ligand in the organic phase between pH 2.0 and 2.5. This result is indicative of the formation of [Cu2(L20)2(SO4)2]. Conventional salicylaldoximes are “strong” copper extractants which require concentrated acid electrolyte to efficiently strip the copper from the organic phase. However, as the use of concentrated acid affects the quality of the copper cathodes, oxygen-containing equilibrium modifiers are often added. These facilitate copper stripping without adversely affecting the loading. The affect of 2-ethylhexanol (2- EH) and trioctylphosphine oxide (TOPO) on the extractive ability of 5-toctylsalicylaldoxime (19) in n-heptane is reported. Both are found to decrease copper extraction more under stripping conditions than loading conditions. 2-EH shows little affect at pH greater than 2.5. TOPO does not significantly affect copper loading at pH greater than 3.0. Evidence for the formation of the adduct [Cu(19-H)2)(TOPO)] was obtained from UV/Vis, IR, EPR and sonic spray mass spectrometry.

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Pavón, Regaña Sandra. "Rare earth elements recovery from E-wastes by solvent extraction and supported liquid membrane processes." Doctoral thesis, Universitat Politècnica de Catalunya, 2019. http://hdl.handle.net/10803/671107.

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Nowadays, rare earth elements (REEs) have gained importance due to their indispensable and critical use in many high-tech industries like hybrid cars, fluorescent lamps, flat screen televisions, mobile phones, disc drives and wind turbines. Since these metals are needed to supply the required functionality in advanced technologies development and the lack of alternative materials, the REEs recovery from urban mining seems to be promising. Moreover, being the ores mines and their strip mining to REEs production placed in a few specific countries such as China, United States and Australia, the stable supply of such metals is becoming a concern. The absence of economical and operational primary deposits in other territories is making many countries consider the REEs recycling from pre-consumer scrap, industrial residues and end-of life products. However, about only 12.5% of e-waste is currently being recycled for all metals due to technological problems, inefficient collection and a lack of incentives and pilot-scale feasible testing to be industrially implemented. In this thesis, different routes to recover and separate these elements from end-of-life products like NdFeB magnets and fluorescent lamps have been developed considering the relevance of these applications in the REEs field and the feasibility of the complete industrial implementation. Regarding NdFeB magnet, it was demonstrated that Nd, the most REE representative component found in magnet wastes, was separated from an Nd/Tb/Dy mixture by using solvent extraction process and intensified processes like liquid membranes in flat sheet configuration. To avoid the inter-step pH conditioning in a continuous industrial process when cationic extractants are used, an ionic liquid such as Primene 81R.Cyanex 572 was proposed in an industrial counter-current extraction process. The results disclosed that two stages were required to separate Nd from the mixture with a purity of 99.7% removing =99% of the initial Tb and Dy. Although both cationic extractants, Cyanex 272 and Cyanex 572, were able to separate the Nd, the transport through the liquid membrane using the former is about 35% slower than using Cyanex 572. Hence, to obtain similar results to those got with Cyanex 572, the membrane area or the working time should be increased when Cyanex 272 is used. REEs from fluorescent lamp wastes were recovered and selectively separated with purities =99.9% by using a process that can be industrially implemented and combines acidic leaching treatments, liquid membranes and cross-flow solvent extraction process. Two successive acidic leachings were needed: (L1) to remove the Ca avoiding its precipitation in following stages of the process and (L2) to recover the REEs present in the waste. Unfortunately, a REEs amount, mainly Y and Eu, was also dragged in the liquid fraction from L1 and these REEs were recovered using Cyanex 923 as carrier by a hollow fibre renewal liquid membrane module. Furthermore, a transport modelling was developed to foresee the permeability coefficient values for Y and Eu depending on the organic solution viscosity and the membrane characteristic parameters. A mathematical modelling was developed using D2EHPA to predict the Y/Eu/Ce mixture extraction behaviour to investigate the optimal separation conditions of the REEs found in the leachate coming from the L2. Once the REEs behaviour was studied in the extraction modelling, the recovery and separation of the REEs were experimentally achieved obtaining purities =99% by four stages cross-flow solvent extraction process using two ionic liquids, Primene 81R.02EHPA and Primene 81R.Cyanex 572. In this sense, REEs recycling processes of both wastes promote potential circular economy based on solutions where a waste is turned into a resource.
Hoy en día, las tierras raras han ganado importancia debido a su uso indispensable y crítico en industrias de alta tecnología. Estos metales son necesarios para el desarrollo de tecnologías avanzadas, lo que hace junto con la falta de materiales alternativos que la recuperación de estos metales de minas urbanas sea prometedora. Por otro lado, las minas y la explotación de este tipo de materiales se encuentran ubicadas en países como China, Estados Unidos y Australia, por lo que el suministro estable de tales metales se está convirtiendo en una preocupación. Ante esta perspectiva, muchos países están considerando seriamente la posibilidad de reciclar tanto los residuos industriales como los productos al final de su vida útil. Sin embargo, en la actualidad sólo se recicla alrededor del 12.5% de los residuos electrónicos, debido principalmente a factores tales como: problemas tecnológicos, ineficiencia en la recolección, falta de incentivos, así como la realización de pruebas viables a escala piloto para su aplicación industrial. En esta tesis se han desarrollado diferentes vías para recuperar y separar estos elementos de productos al final de su vida útil, centrándose principalmente en los imanes de NdFeB y las lámparas fluorescentes, teniendo en cuenta su reciente importancia en el campo de las tierras raras y la viabilidad de la implementación industrial. En los trabajos realizados con imanes de NdFeB, se demostró que el Nd se puede separar de una mezcla de NdfTb/Dy mediante extracción líquido-líquido y procesos más intensivos como las membranas líquidas en configuración de lámina plana. Tratando de evitar el acondicionamiento del pH entre etapas en un proceso industrial continuo usando extractantes catiónicos, se propuso trabajar con un líquido iónico como el Primene 81R.Cyanex 572. Se necesitaron dos etapas en la separación de Nd de la mezcla con una pureza del 99.7%, eliminando = 99% de Tb y Dy inicial a través de un proceso de extracción a contracorriente. El transporte a través de la membrana líquida usando Cyanex 272 fue aproximadamente 35% más lento que usando Cyanex 572. Por lo tanto, el área de la membrana o el tiempo de trabajo debería aumentarse cuando se utiliza el primero para obtener resultados similares a los obtenidos con Cyanex 572. Las tierras raras de los residuos de lámparas fluorescentes se recuperaron y separaron selectivamente con purezas = 99.9% mediante un proceso que puede ser implementado industrialmente y que combina tratamientos de lixiviación ácida, membranas líquidas y extracción de flujo cruzado. Se necesitaron dos tratamientos de lixiviación: (L1) para eliminar el calcio evitando su precipitación en las siguientes etapas del proceso y (L2) para recuperar las tierras raras presentes en los residuos. Desafortunadamente, una cantidad de estos metales, principalmente Y y Eu, también fue lixiviada en L1. Éstos fueron recuperados utilizando un módulo de fibra hueca con renovación de la membrana líquida usando Cyanex 923 como portador. Se desarrolló un modelo de transporte para prever los valores del coeficiente de permeabilidad para Y y Eu dependiendo de la viscosidad de la solución orgánica y de los parámetros característicos del soporte de la membrana. Además, se desarrolló un modelo matemático usando D2EHPA para predecir el comportamiento de extracción de la mezcla Y/Eu/Ce para investigar la extensión de la separación de estos metales presentes en el lixiviado del L2. Una vez estudiado el comportamiento de estas tierras raras, se logró la recuperación y separación obteniendo purezas =99% por medio de un proceso de extracción líquido-líquido de flujo cruzado en cuatro etapas utilizando Primene 81R.02EHPA y Primene 81R.Cyanex 572. En este sentido, los procesos de reciclaje de tierras raras desarrollados para ambos residuos promueven una economía circular potencial basada en soluciones en las que un residuo se convierte en un recurso

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SOARES, PAULO S. M. "Estudo preliminar do fracionamento de terras raras medias e pesadas em grupos com extracao por solventes." reponame:Repositório Institucional do IPEN, 1994. http://repositorio.ipen.br:8080/xmlui/handle/123456789/10353.

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IPEN/D
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

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FAVARO, DEBORA I. T. "Estudo do comportamento de alguns lantanidios nas extracoes com misturas binarias de acido DI-(2-ETILHEXIL) fosforico (HDEHP) tenoiltrifluoroacetona." reponame:Repositório Institucional do IPEN, 1985. http://repositorio.ipen.br:8080/xmlui/handle/123456789/9843.

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Tese (Doutoramento)
IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

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Negrete-Virgen, Juan Alejandro. "Manufacture of adenoviral vectors for gene therapy applications : critical comparison of solvent extraction and adsorption-based processes." Thesis, University of Birmingham, 2003. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.288887.

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The biotechnology industry has recently been demanding nanoparticulate products (20-200 nm) such as viruses, plasmids, virus-like particles and drug delivery assemblies. These products are mainly used as gene delivery systems in gene therapy protocols. Adenoviral vectors {Ad) are the most exploited gene therapy vectors in industry worldwide. The :ma.nu.fu.cture of Ad fuces several problems including {i) small volumes of product per batch of cell culture, {ii) inaccurate, time consuming and multifuctor-dependant methods for infectivity determination and (iii) downstream processing. The downstream processing requires methods to purify infective particles :from the contaminants including non-infective particles, partially assembled particles, :free adenoviral components, host cell components and medium components. The solvent extraction method, aqueous two-phase systems {ATPS) and selective chromatography can potentially circumvent such downstream processing problems. ATPS has been applied to the purification of soluble macromolecular products. However, the recovery of nanoparticles represents a practical constraint due to their partition in the interphase. Selective chromatography has been also a method for high performance purification of bioproducts. However, in the context of nanoparticulates, product and contaminants adsorb and desorb (i.e. copurify) under similar mobile phase conditions due to sheared chemistry. In this study, infective Ad were concentrated in the top phase of a polymer-salt ATPS. Additionally, the potential ATPS miniaturisation for scouting experiments was evaluated. The infective Ad were also partially purified exploiting a fluidised bed. In this process, an anionexchange commercial adsorbent laminated with electrophoretic grade neutral agarose was utilised. The porosity of the pellicle was designed to exclude Ad yet fucilitate diffusion of macromolecular components to adsorption sites within the interior of the adsorbent core (subtractive adsorption). Furthermore, a method for monitoring infective Ad with rapid and easy handling by means of flow cytometric analysis was developed. In order to perform the experiments, the Ad production was scaled-up to a 2 L bioreactor. The recovery processes evaluated in this study and conclusion drown will contribute to the recovery of Ad but also could be applied to recover other nanoparticulate bioproducts

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ZARPELON, LIA M. C. "Contribuicao ao estudo da separacao zirconio/hafnio no sistema MIBK-HSCN-HCL." reponame:Repositório Institucional do IPEN, 1995. http://repositorio.ipen.br:8080/xmlui/handle/123456789/10423.

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IPEN/D
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

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Turkington, Jennifer Rachel. "Investigation into the modes of action of extractants for base metal cations and metalate anions." Thesis, University of Edinburgh, 2013. http://hdl.handle.net/1842/9567.

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This thesis involves the design and development of reagents for the recovery of base metals (specifically zinc, nickel and cobalt) in hydrometallurgical solvent extraction processes. The work aims to demonstrate how ligand design can affectively tune the strength and selectivity of extractants to achieve efficient recovery of the desired base metals. Chapter 1 reviews current solvent extraction processes used in extractive metallurgy, encompassing both the well established technologies developed for sulfate streams as well as those more recently explored for treating chloride streams. Also reviewed, is the nature of the chemical binding involved in the three key modes of extraction; namely cation transport, anion transport and metal salt transport. Chapter 2 summarises the methodologies that have been established during this research for the appropriate testing of these reagents. Chapter 3 deals exclusively with the processing of zinc sulfide ores with an aim to design reagents to achieve concentration and separation of zinc in chloride hydrometallurgical circuits. The amido functionalised reagents that are reported have a common structural feature with ligands that have been previously studied by the Tasker group (Ross J. Ellis Thesis, University of Edinburgh, 2009). A six membered chelate ring is formed by a protonated amino nitrogen atom and an amido oxygen atom in a sequence of the type R2HN+-CH2-NR-CO-R. This differs from those previously studied which have a sequence of the type R2HN+-CH2-CHR-CO-NR2. The pro-ligands (L) operate via an anion exchange mechanism (Equation 1) whereby two protonated ligands (LH+) coordinate to the outersphere of anionic zinc(II) or iron(III) chloridometalates from acid chloride solutions using both N-H and C-H hydrogen-bond donors. pH dependent solvent extraction experiments have concluded that this reagent series achieves zinc(II) loading with pH0.5 values that are competitive with the previous ligand series (Ross J. Ellis Thesis, University of Edinburgh, 2009). Chloride concentration dependent solvent extraction experiments have demonstrated that the reagents show an unusually good selectivity for ZnCl4 2- over chloride or FeCl4 - in equilibrium of the type; yLorg + yH+ +MClx y- ⇌ [(LH)yMClx](org) (1) The development of bidentate and tridentate pyrazolone-based pro-ligands for the extraction of nickel and cobalt from mixed metal sulfate streams is considered in Chapters 4 and 5. These reagents (LH) operate via metal cation transport, where an inner-sphere complex of nickel(II) or cobalt(II) is formed with the ligand (L-) see Equation 2. A combination of N, O and S donors has been incorporated into 1-phenyl-3-methyl-4- acylpyrazol-5-ones and their respective 4-acylpyrazolone oximes in order to tune the bidentate ligands (L-) for optimal coordination with nickel(II) or cobalt(II). Substituent effects have also been investigated, by synthesising a series of 1-(2-X-phenyl)-3-methyl-4- acylpyrazol-5-one oximes [X = Cl, H]. Substitution in the 3-position of the phenol group in phenolic oximes has been reported to increase extractant strength for copper by two orders of magnitude (Ross S. Forgan Thesis, University of Edinburgh, 2008). Similar improvements were not observed in this study. The nature of this effect has been attributed to buttressing of hydrogen-bonds, where the substituent forms a stabilising, bifurcated hydrogen-bond between the oximic hydrogen and the pyrazolonic oxygen. yLHorg + My+ ⇌ [(L)yM]org + yH+ (2) Tridentate analogues of the oxime reagents above have been prepared as imines derived from anilines contained o-O, S or N donor atoms. It was hoped that these would give high spin octahedral nickel(II) complexes in extraction processes. They proved to be weak extractants. Chapter 6 focuses of the development of bidentate pyrazolethiones for the selective extraction of cobalt from manganese in acidic sulfate streams. These reagents have been designed to favour coordination to metals in a tetrahedral geometry as shown by L. Emeleus and A. Smith for copper and zinc (Lucy Emeleus Thesis, University of Edinburgh 1999 and Andrew Smith Thesis, University of Edinburgh 2000).

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SANTOS, JACINETE L. dos. "Recuperacao de ions Eu(III) e de U(VI) de efluentes aquosos utilizando a tecnica de membranas liquido suportadas (MLS) e macrociclicos como agentes extratores." reponame:Repositório Institucional do IPEN, 2007. http://repositorio.ipen.br:8080/xmlui/handle/123456789/9379.

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Tese (Doutoramento)
IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

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Ramirez, Cadavid David A. "Development of Processes for the Extraction of Industrial Grade Rubber and Co-Products from the Roots of Taraxacum kok-saghyz (TK)." The Ohio State University, 2017. http://rave.ohiolink.edu/etdc/view?acc_num=osu1512060296142347.

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Lundstedt, Staffan. "Analysis of PAHs and their transformations products in contaminated soil and remedial processes." Doctoral thesis, Umeå universitet, Kemi, 2003. http://urn.kb.se/resolve?urn=urn:nbn:se:umu:diva-57.

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Soil that is heavily contaminated with polycyclic aromatic hydrocarbons (PAHs) is often found at the sites of former gasworks and wood-impregnation plants. Since PAHs are toxic these sites represent a hazard to human health and the environment, and therefore they need to be treated, preferably by a method that destroys the contaminants, and thus eliminates the problem permanently. However, during biological and chemical degradation of PAHs other toxic compounds may be formed. If these transformation products are sufficiently persistent they could potentially accumulate during remedial processes. In the work underlying this thesis the degradation and transformation of PAHs were studied in three remedial processes: viz. a pilot-scale bioslurry reactor, microcosms with wood-rotting fungi and lab-scale treatments with Fenton's reagent. A group of transformation products referred to as oxygenated-PAHs (oxy-PAHs) was found to be particularly important, as these compounds are toxic and were shown to be relatively persistent in the environment. The oxy- PAHs were, for instance, found at significant concentrations in the gasworks soil used in most of the studies. This soil was highly weathered and had therefore been depleted of the more readily degradable compounds. In addition, experiments in which earthworms were exposed to the gasworks soil showed that the oxy-PAHs were more easily taken up in living organisms than PAHs. To facilitate the studies, new extraction and fractionation methods were developed. For instance, pressurized liquid extraction (PLE) was investigated for its reliability and efficiency to extract PAHs and oxy-PAHs from soil. Furthermore, a selective PLE-method was developed that can simultaneously extract and separate the PAHs and oxy-PAHs into two different fractions. This was accomplished by adding a chromatographic material (silica or Florisil) to the extraction cell. Under certain conditions all three remedial processes resulted in increasing amounts of oxy- PAHs in the soil. For example, 1-acenaphthenone and 4-oxapyrene-5-one accumulated in the bioslurry reactor. Similarly, in the soil inoculated with a white-rot fungus 9-fluorenone, benzo[a]anthracene-7,12-dione, 4-hydroxy-9-fluorenone and 4-oxapyrene-5-one accumulated. Finally, in an ethanol-Fenton treatment the concentration of some PAH-quinones increased in the soil. The results show that it might be necessary to monitor oxy-PAHs as well as PAHs during the remediation of PAH-contaminated sites. Otherwise, the soil may be considered detoxified too early in the process. In the long term it would be desirable to include analyses with sufficient marker compounds to follow the possible production and elimination of the oxy-PAHs. However, until such compounds can be identified it is suggested that contaminated soil should be screened for oxy-PAHs in general. The selective PLE-method presented in this thesis could be a useful tool for this.

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Makaka, Siphokazi. "The development of an empirical mass transfer relationship for the extraction of copper ions in a carrier facilitated tubular supported liquid membrane system." Thesis, Cape Peninsula University of Technology, 2011. http://hdl.handle.net/20.500.11838/866.

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Thesis submitted in fulfilment of the requirements for the degree Master of Technology: Chemical Engineering in the Faculty of Engineering at the Cape Peninsula University of Technology 2011
Treatment of waste material from mining and mineral processing is gaining increasing importance as a result of the increasing demand for high purity products and environmental concerns. Supported liquid membranes (SLMs) have been proposed as a new technology for the selective removal of metal ions from a solution. This technology can be described as the simultaneous extraction and stripping operation, combined in a continuous single process unit. Theoretically, the rate of mass transfer through SLM systems could be controlled by three resistances, namely: · Resistance through the feed-side · Resistance through the strip-side laminar layers; and · Diffusion through the membrane. It has been reported that transport resistance in the feed-side laminar layer is controlling. (Srisurichan et al, 2005:186). The objective of this research was to extract copper ions in a TSLM system, evaluate the effect of the feed characteristics on the feed-side laminar layer and determine a relationship between the applicable dimensionless numbers, i.e. Sherwood, Schmidt and Reynolds numbers. A Counter-current, double pipe Perspex bench-scale reactor, consisting of a single hydrophobic PVDF tubular membrane mounted vertically within, was used for the test work. The membrane was impregnated with LIX 984N-C and became the support for this organic transport medium. Dilute Copper solution passed through the centre pipe and sulphuric acid, as a strippant, passed through the shell side. In this test work, Copper was successfully transported from the feed-side to the strip-side and through repetitive results; a relationship between dimensionless numbers was achieved.

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Khalfalla, Hamza Abdulmagid. "Modelling and optimisation of oxidative desulphurization process for model sulphur compounds and heavy gas oil : determination of rate of reaction and partition coefficient via pilot plant experiment : modelling of oxidation and solvent extraction processes : heat integration of oxidation process : economic evaluation of the total process." Thesis, University of Bradford, 2009. http://hdl.handle.net/10454/4247.

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Heightened concerns for cleaner air and increasingly more stringent regulations on sulphur content in transportation fuels will make desulphurization more and more important. The sulphur problem is becoming more serious in general, particularly for diesel fuels as the regulated sulphur content is getting an order of magnitude lower, while the sulphur contents of crude oils are becoming higher. This thesis aimed to develop a desulphurisation process (based on oxidation followed by extraction) with high efficiency, selectivity and minimum energy consumption leading to minimum environmental impact via laboratory batch experiments, mathematical modelling and optimisation. Deep desulphurization of model sulphur compounds (di-n-butyl sulphide, dimethyl sulfoxide and dibenzothiophene) and heavy gas oils (HGO) derived from Libyan crude oil were conducted. A series of batch experiments were carried out using a small reactor operating at various temperatures (40-100 °C) with hydrogen peroxide (H2O2) as oxidant and formic acid (HCOOH) as catalyst. Kinetic models for the oxidation process are then developed based on 'total sulphur approach'. Extraction of unoxidised and oxidised gas oils was also investigated using methanol, dimethylformamide (DMF) and N-methyl pyrolidone (NMP) as solvents. For each solvent, the 'measures' such as: the partition coefficient (KP), effectiveness factor (Kf) and extractor factor (Ef) are used to select the best/effective solvent and to find the effective heavy gas oil/solvent ratios. A CSTR model is then developed for the process for evaluating viability of the large scale operation. It is noted that while the energy consumption and recovery issues could be ignored for batch experiments these could not be ignored for large scale operation. Large amount of heating is necessary even to carry out the reaction at 30-40 °C, the recovery of which is very important for maximising the profitability of operation and also to minimise environmental impact by reducing net CO2 release. Here the heat integration of the oxidation process is considered to recover most of the external energy input. However, this leads to putting a number of heat exchangers in the oxidation process requiring capital investment. Optimisation problem is formulated using gPROMS modelling tool to optimise some of the design and operating parameters (such as reaction temperature, residence time and splitter ratio) of integrated process while minimising an objective function which is a coupled function of capital and operating costs involving design and operating parameters. Two cases are studied: where (i) HGO and catalyst are fed as one feed stream and (ii) HGO and catalyst are treated as two feed streams. A liquid-liquid extraction model is then developed for the extraction of sulphur compounds from the oxidised heavy gas oil. With the experimentally determined KP multi stage liquid-liquid extraction process is modelled using gPROMS software and the process is simulated for three different solvents at different oil/solvent ratios to select the best solvent, and to obtain the best heavy gas oil to solvent ratio and number of extraction stages to reduce the sulphur content to less than 10 ppm. Finally, an integrated oxidation and extraction steps of ODS process is developed based on the batch experiments and modelling. The recovery of oxidant, catalyst and solvent are considered and preliminary economic analysis for the integrated ODS process is presented.

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Manic, Marina. "Alternative solvents in separation processes." Doctoral thesis, Faculdade de Ciências e Tecnologia, 2012. http://hdl.handle.net/10362/8774.

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Dissertation presented to obtain the Ph.D degree in Sustainable Chemistry
Fundação para a Ciência e Tecnologia - through doctoral fellowship SFRH/BD/45323/2008, and grant No Pest-C/EQB/LA0006/2011; partially supported from the Conselho de Reitores das Universidades Portuguesas (CRUP) – Integrated project Portugal-Spain, No E-95/10.

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Van, Dyk Braam. "Computerized design of solvents for extractive processes." Thesis, Stellenbosch : Stellenbosch University, 2001. http://hdl.handle.net/10019.1/52171.

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Thesis (PhDEng)--University of Stellenbosch, 2001.
ENGLISH ABSTRACT: Separation processes are an integral part of chemical engineering. The purity of a chemical product is among the principal factors influencing its value. Therefore, any method that can increase the purity of a product or decrease the cost of purification will have a direct effect on the profitability of the entire plant. An important class of separation processes is the solvent-based separations. This includes processes like extractive distillation, liquid-liquid extraction and chromatographic separation. Heterogeneous azeotropic distillation is closely related to these processes. The most important variable in the design of a solvent-based separation process is the choice of solvent. A genetic algorithm for the computer-aided molecular design of solvents for extractive distillation had been previously developed by the author. This algorithm was improved and expanded to include liquid-liquid extraction, heterogeneous azeotropic distillation, gas-liquid chromatography and liquid-liquid (partition) chromatography. At the same time the efficiency of the algorithm was improved, resulting in a speed increase of up to 500% in certain cases. An automatic parameter tuning algorithm was also implemented to ensure maximum efficiency of the underlying genetic algorithm. In order to find suitable entrainers for heterogeneous azeotropic distillation a method is required to locate any ternary heterogeneous azeotropes present in a system. A number of methods proposed in the literature were evaluated and found to be computationally inefficient. Two new methods were therefore developed for ternary systems. A methodology for applying these methods to quaternary and higher systems was also proposed. Two algorithms to design blended solvents were also developed. Blended solvents allow the use of simpler and thus cheaper solvents by spreading the active functional groups over several molecular backbones. It was observed in a number of cases that the blended solvents performed better than their individual components. This was attributed to synergistic interactions between these components. Experimental evidence for this effect was also found. The algorithm was applied to a number of industrially important separation problems, including the extremely difficult final purification process of alpha olefins. In each case solvents were found that are predicted to perform substantially better than those that are currently used in industry. A number of these predictions were tested by experiment and found to hold true.
AFRIKAANSE OPSOMMING: Skeidingsprosesse is 'n integrale deel van chemiese ingenieurswese. Die suiwerheid van 'n chemiese produk is een van die hoof faktore wat die waarde daarvan bepaal. Derhalwe sal enige metode wat die suiwerheid van 'n produk kan verbeter, of die koste van die suiwering daarvan kan verlaag, 'n direkte effek op die winsgewendheid van die hele aanleg hê. 'n Belangrike groep skeidingsprosesse is die oplosmiddel-gebaseerde skeidings. Dit sluit prosesse soos ekstraktiewe distillasie, vloeistofvloeistof ekstraksie en chromatografiese skeidings in. Heterogene azeotrope distillasie is nou verwant aan hierdie prosesse. Die belangrikste veranderlike in die ontwerp van so 'n oplosmiddel-gebaseerde proses is die keuse van oplosmiddel. 'n Genetiese algoritme vir die rekenaargesteunde molekulêe ontwerp van oplosmiddels vir ekstraktiewe distillasie is voorheen ontwikkel deur die skrywer. Hierdie algoritme is verbeter en uitgebrei om vloeistofvloeistofekstraksie, heterogene azeotrope distillasie, gas-vloeistof chromatografie en vloeistof-vloeistof (verdelings) chromatografie in te sluit. Ter selfde tyd is die doeltreffendheid van die algoritme verbeter, wat 'n verbetering in spoed van tot 500% in sekere gevalle tot gevolg gehad het. 'n Algoritme om die parameters van die onderliggende genetiese algoritme outomaties te verfyn is ook geïm plementeer om die optimale werksverrigting van die algoritme te verseker. Om gepaste saamsleepmiddels vir heterogene azeotrope distillasie te vind, word 'n metode benodig om enige ternêre heterogene azeotrope aanwesig in 'n stelsel op te spoor. 'n Aantal sulke metodes wat in die literatuur voorgestel is, is geëvaluEer en daar is gevind dat hierdie metodes ondoeltreffend is. Twee nuwe metodes is derhalwe ontwikkel vir ternêre stelsels. 'n Metodiek om hierdie metodes op kwaternêre en hoër stelsels toe te pas, is ook voorgestel. Twee algoritmes vir die ontwerp van gemengde oplosmiddels is ook ontwikkel. Gemengde oplosmiddels laat die gebruik van eenvoudiger en dus goedkoper oplosmiddels toe, deur die aktiewe funksionele groepe oor 'n aantal molekulêe strukture te versprei. Daar is 'n aantal gevalle waargeneem waar die mengsel beter skeiding bewerkstellig het as die individuele oplosmiddels waaruit dit bestaan. Dit is toegeskryf aan 'n sinergistiese wisselwerking tussen die komponente van die mengsel. Eksperimentele getuienis vir hierdie effek is ook ingewin. Die algoritme is toegepas op 'n aantal belangrike skeidingsprobleme vanuit die bedryf, insluitende die uiters moeilike finale suiwering van alfa olefiene. In elke geval is oplosmiddels gevind wat volgens voorspelling aansienlike beter skeidings sal bewerkstellig as dié wat tans in die bedryf gebruik word. 'n Aantal van hierdie voorspellings is eksperimenteel getoets en korrek bewys.

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Machado, Alex Barreto. "Estudos do processo de extração liquido-liquido para a purificação do acido acrilico." [s.n.], 2007. http://repositorio.unicamp.br/jspui/handle/REPOSIP/267256.

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Orientadores: Maria Regina Wolf Maciel, Martin Aznar
Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Quimica
Made available in DSpace on 2018-08-11T22:03:29Z (GMT). No. of bitstreams: 1 Machado_AlexBarreto_M.pdf: 1251594 bytes, checksum: 12614335c44f56e98288ed9de32033db (MD5) Previous issue date: 2007
Resumo: Observa-se que, nos últimos anos, a procura por novos processos de separação para a recuperação de ácidos orgânicos, dentre eles o ácido acrílico, a partir de seu caldo de fermentação, tem sido intensa. O processo de extração líquido-líquido apresenta-se como uma alternativa das mais viáveis para sistemas diluídos, quando se utiliza solventes apropriados e de baixa toxicidade. Na parte computacional do trabalho em questão, inicialmente, realizou-se um estudo do software Aspen Plus no que se refere à obtenção de dados termodinâmicos (parâmetros binários) e curvas binodais. Realizou-se, também, a validação do software obtendo regressões de dados experimentais envolvendo fenol e alguns solventes retirados da literatura. Algumas curvas de extração (curvas binodais), testando diferentes solventes para extração do ácido acrílico, foram construídas. As curvas binodais simuladas no Aspen também auxiliaram na escolha dos pontos experimentais, uma vez que, desta maneira, já se conhecia a região de formação de duas fases dos sistemas em estudo e pôde-se orientar a coleta destes dados laboratoriais sem o consumo excessivo de reagentes e de tempo. A parte experimental deste projeto envolve a obtenção de dados de ELL dos sistemas ternários ácido acrílico - água e os seguintes solventes: diisopropil éter, isopropil acetato, 2-etil 1-hexanol, 4- metil 2-pentanona; além do levantamento dos dados de ELL dos sistemas quaternários: ácido acrílico+água+diisopropil éter+sal, usando como sais MgCl2 e CaCl2 de concentrações de 5 e 10%, respectivamente, e ácido acrílico+água+isopropil acetato+sal, usando como sais MgCl2 e CaCl2 de concentrações de 5 e 10% respectivamente. Os resultados encontrados foram muito satisfatórios, permitindo-se construir curvas de solubilidades e realizar as regressões utilizando os modelos de coeficiente de atividade UNIQUAC e NRTL, determinando-se os parâmetros binários. Foram realizadas comparações entre os 4 solventes de extração e entre os sistemas quaternários envolvendo sais.
Abstract: It is observed that, in the last years, the search for new separation processes for recovering organic acids, such as acrylic acid produced from renewable sugar, has been intense. The liquid-liquid extraction process appears as the most viable alternative for diluted systems, since suitable solvents are used. Related to the computational part of this work, initially, a study using the software Aspen Plus for obtaining thermodynamic data (binary parameters) and binodal curves were carried out. Some extraction curves (binodal curves), testing different solvents for acrylic acid extraction, were obtained. Binodal curves simulated with Aspen Plus were very important in choosing experimental points, since, in this way, it was possible to know the region where there are immiscible two phases and, so, to facilitate the obtention of experimental data without excessive consumption of reagents and time. In the experimental section of this work, experimental data of liquid liquid equilibria (LLE) were obtained for the ternary systems acrylic acid + water + solvents (diisopropyl ether, isopropyl acetate, 2-ethyll 1-hexanol, 4 - methyl 2-pentanona), beyond obtain LLE data for the quaternary systems acrylic acid + water + diisopropyl ether + salt (using MgCl2 or CaCl2, with concentrations of 5 and 10%, respectively) and system acrylic acid + water + isopropyl acetate + salt (using MgCl2 and CaCl2 with concentrations of 5 and 10%, respectively). The results obtained were very satisfactory. Experimental solubility curves and regressed curves, using UNIQUAC and NRTL models for the activity coefficient calculations, through the binary parameters, were carried out. The results obtained with four solvents were compared and the ternary and quaternary systems (involving salts) also were compared among themselves.
Mestrado
Desenvolvimento de Processos Químicos
Mestre em Engenharia Química

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18

Alberts, Estelle. "Stripping rare earth elements and iron from D2EHPA during zinc solvent extraction." Thesis, Stellenbosch : Stellenbosch University, 2011. http://hdl.handle.net/10019.1/17999.

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Thesis (MScEng)--Stellenbosch University, 2011.
ENGLISH ABSTRACT: At Skorpion Zinc mine, in south-west Namibia, zinc oxide ore is refined through sulphuric acid leaching, solvent extraction, electrowinning and casting of the final 99.995 % Zn metal. Over the last four years, the rare earth element concentrations, with particular reference to Y, Yb, Er and Sc, have significantly increased in the circulating electrolyte and the zinc-stripped organic phase streams in the electrowinning and solvent extraction processes. This project had two main objectives: firstly, the effect(s) of rare earths on the zinc solvent extraction and electrowinning processes were to be determined; based on these results, the second objective was to find a suitable method for removing rare earth elements from the organic phase during zinc solvent extraction. The investigation into the effect of the rare earths on zinc electrowinning showed that an increase of 100 mg/l in the electrolyte Y concentration caused a decrease of 6 % in current efficiency. The elemental order of decreasing current efficiency was found to be: Y > Yb > Er > Sc. In the zinc solvent extraction process, it was found that an increase in the total organic rare earth elements and iron concentration from 3100 to 6250 mg/l resulted in doubled viscosity and an increase in phase disengagement time from 100 to 700 seconds. The organic zinc loading capacity after two extraction stages was reduced by 1 – 3 g/l depending on the pregnant leach solution used. The detrimental effect of rare earth elements on solvent extraction and electroplating of zinc therefore justified the development of a rare earth element removal process. Stripping of low concentrations of rare earth elements from 40% D2EHPA diluted in kerosene to produce a clean organic for zinc extraction was investigated using bench-scale experiments in a glass jacketed mixing cylinder. For the rare earths, the best stripping agent was found to be H2SO4, followed by HCl and then HNO3. Hydrochloric acid achieved better Fe stripping than sulphuric acid. Acid concentration was tested in the range of 1 to 7 M, organic-to-aqueous ratio for the range of 0.25 to 6.0 and temperatures between 30 and 55 °C. More than 80% stripping of yttrium and erbium could be achieved at an optimum hydrochloric acid concentration of 5 M and more than 90% rare earth element (specifically Y, Er, Yb) stripping from the organic phase could be achieved with 5 M sulphuric acid. Stripping was improved by reducing the organic-to-aqueous ratio to as low as 0.5 and increasing the temperature. Stripping increased with increasing temperature in an S-shaped curve, flattening off at 50°C. The effect of O:A ratio was more significant than the effect of temperature on rare earth stripping. The results showed good repeatability, and were not limited by the rare earth concentration, agitation rate or equilibrium time in the range of set points used in the experiments. Statistical models were compiled to fit the experimental data obtained for Y, Yb, Er and Fe when stripped with sulphuric and hydrochloric acid respectively. All models showed dependence on the acid concentration and squared-concentration and interaction effects between the O:A ratio and temperature and stripping agent concentration were significant. The models were compiled for the experimental data obtained from stripping synthetically prepared organic and then tested on results obtained when stripping the plant organic phase. The following three process solutions were discussed for implementation on a plant scale for the removal of rare earths from the organic phase during zinc solvent extraction: Sulphuric acid stripping mixer settler or stripping column, improvement of available HCl stripping section and replacement of the organic inventory. The possibility of an oxalic acid precipitation process to obtain value from the rare earths as by-product was also discussed. It was concluded that the current process that uses HCl to strip off iron and rare earths would be the best practically and financially feasible process. Value can be gained from the rare earths if a rare earth element - oxalic acid precipitation section that is financially feasible can be established.
AFRIKAANSE OPSOMMING: By Skorpion Zinc myn, in suidwes Namibië, word sinkoksied erts gesuiwer deur middel van swaelsuur-loging, oplosmiddel ekstraksie, elektroplatering en gieting van die finale 99.995 % Zn metaal. Oor die afgelope vier jaar het die seldsame aardmetale konsentrasie, spesifiek Y, Yb, Er en Sc, noemenswaardig in die sirkulerende elektroliet en sink-gestroopte organiese fase toegeneem. Hierdie projek het twee hoofdoelstellings gehad: eerstens moes die effek van seldsame aardmetale op die sink oplosmiddel ekstraksie en elektroplatering prosesse bepaal word; gebaseer op hierdie resultate, was die tweede doelstelling om ‘n geskikte metode vir die verwydering van seldsame aardmetale vanaf die organiese fase gedurende sink oplosmiddel ekstraksie te vind. Die ondersoek na die effek van seldsame aardmetale op sink elektroplatering het gewys dat ‘n verhoging van 100 mg/l in die elektroliet Y konsentrasie ‘n verlaging van 6 % in kragdoeltreffendheid veroorsaak het. Die element-orde van verminderende kragdoeltreffendheid was Y > Yb > Er > Sc. Vir die sink oplosmiddel ekstraksie proses, is gevind dat ‘n verhoging in die totale organiese seldsame aardmetaal- en yster konsentrasie van 3100 tot 6250 mg/l ‘n verdubbelde viskositeit en ‘n verlenging in faseskeidingstyd van 100 tot 700 sekondes tot gevolg gehad het. Die organiese sink ladingskapasiteit na twee ekstraksie stappe is met 1 – 3 g/l verminder afhangende van die logings oplossing wat gebruik is. Die nadelige effek van seldsame aardmetale op oplosmiddel ekstraksie en sink elektroplatering het die ontwikkeling van ‘n seldsame aardmetale verwyderingsproses regverdig. Die verwydering van lae konsentrasies seldsame aardmetale vanaf die D2EHPA-keroseen organiese fase om ‘n skoon organiese fase vir sink-ekstraksie te verkry is ondersoek deur banktoetsskaal eksperimente. Vir die seldsame aardmetale is bevind dat H2SO4 die beste stropingsagent is, gevolg deur HCl en dan HNO3. Soutsuur het beter yster verwydering as swaelsuur bewerkstellig. Suurkonsentrasies van 1 tot 7 M, O:A verhoudings van 0.25 tot 6 en temperature tussen 30 en 55°C is getoets. Meer as 80% verwydering van yttrium en erbium kon bereik word met ‘n optimum HCl konsentrasie van 5 M en meer as 90% seldsame aardmetale (spesifiek Y, Er en Yb) verwydering vanaf die organiese fase met 5 M swaelsuur. Seldsame aardmetale en yster verwydering kon verbeter word deur die organies-tot-waterfase (O:A) verhouding te verminder tot so laag as 0.5 en deur die temperatuur te verhoog. Stroping het in ‘n S-kurwe verhoog soos die temperatuur verhoog het, en het afgeplat teen 50°C. Die effek van die O:A verhouding was belangriker as die effek van temperatuur op stroping. Die resultate het goeie herhaalbaarheid gewys, en is nie deur massaoordrag beperk nie. Statistiese modelle is saamgestel om die eksperimentele data wat vir Y, Yb, Er en Fe verkry is vir stroping met swaelsuur en soutsuur te pas. Al die modelle het afhanklikheid van die suurkonsentrasie en kwadratiese suurkonsentrasie gewys en interaksie effekte tussen die O:A verhouding, temperatuur en suurkonsentrasie was belangrik. Die modelle is saamgestel vir die eksperimentele data wat verkry is vanaf stroping van ‘n sintetiese organiese fase en is toe getoets op resultate wat verkry is vanaf stroping van die aanleg se organiese fase. Die volgende drie proses-oplossings is oorweeg vir implementering op ‘n aanlegskaal vir die verwydering van seldsame aardmetale vanaf die organiese fase gedurende sink oplosmiddel ekstraksie: Swaelsuur stroping menger-afskeidingstenk of stropingskolom, verbetering van die bestaande HCl aanleg en vervanging van die organiese inventaris. ‘n Moontlike oksaalsuur presipitasie proses om waarde vanaf die seldsame aardmetale as by-produk te verkry is ook bespreek. Daar is tot die gevolgtrekking gekom dat die huidige proses wat HCl gebruik om yster en seldsame aardmetale van die organiese fase af te stroop, die beste praktiese en finansieel vatbare proses huidiglik is. Waarde kan vanaf die seldsame aardmetale verkry word as ‘n seldsame aardmetale – oksaalsuur presipitasie afdeling wat finansieel haalbaar is daargestel kan word.

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Olivier, Michiel Casparus. "Developing a solvent extraction process for the separation of cobalt and iron from nickel sulphate solutions." Thesis, Stellenbosch : Stellenbosch University, 2011. http://hdl.handle.net/10019.1/17984.

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Thesis (MScEng)--Stellenbosch University, 2011.
ENGLISH ABSTRACT: Crude NiSO4 solutions are often produced as a product of Sherrit based matte leach processes leading to iron and cobalt contaminated solutions of NiSO4. To upgrade the quality of these solutions for either, the production of NiSO4 crystals or cathode/precipitated nickel, the iron and cobalt must be removed. Conventional processes use either pure or saponified Cyanex 272 in solvent extraction to extract iron and cobalt from pregnant nickel leach solutions. These processes require the addition of an alkali like NaOH to neutralise the protons being exchanged for the different metal species since extraction is a strong function of pH. Hence, while removing iron and cobalt from the solution, sodium is added instead. This limitation can be dealt with by pre-loading of Cyanex 272 with a portion of the purified nickel product prior to impurity extraction. During the extraction stage nickel is then exchanged for the impurities instead of hydrogen and no NaOH addition is necessary, resulting in a pure nickel product. The extracted metals are recovered from the organic phase by stripping it with H2SO4 and the organic phase is recycled. A solvent extraction process that purifies an 80 g/l nickel sulfate solution from 1 g/l cobalt and 3 g/l iron was developed. The key variables include pH, organic/aqueous (O/A) mixing ratio, nickel loading, H2SO4 concentration, Cyanex 272 concentration, various organic diluents and temperature. These variables were investigated via preliminary and three 24 factorial design batch experiments which reduced the variables to pH/NaOH addition and O/A ratio for the pre-loading section, nickel loading and O/A ratio for the extraction section and H2SO4 concentration and A/O ratio for the stripping section. The reduced variables were considered in further batch experiments from which the data was used to develop models and design a simulation sheet in Microsoft Excel of the extraction circuit. These final batch tests revealed the conditions that resulted in the purest aqueous nickel product after extraction, where nickel and cobalt can selectively be stripped from iron and what H2SO4 concentration and A/O ratio is necessary to finally strip iron and regenerate the organic phase. Ultimately four tests were conducted on a mixer-settler setup to test the validity of the simulation sheet. The proposed process conditions for the solvent extraction circuit are to use a 20V% Cyanex 272 solution in Shellsol D70 as diluent that are pre-loaded with an 80 g/l purified nickel product solution at an O/A ratio of 25 and a pH of 7 generating a nickel loading of 3.2 g/l for the extraction section. This loading at an O/A ratio of 1.5 produces a high pure nickel aqueous product (0.05 g/l Co, 0.01 g/l Fe). From the generated organic phase co-extracted nickel and cobalt can selectively be stripped with 0.1 M H2SO4 at an A/O ratio of 2.25 followed by an 1 M H2SO4 solution at an A/O ratio of 0.75 to strip the remaining iron. The temperature at all the stages should be controlled between 40-50°C to ensure phase separation.
AFRIKAANSE OPSOMMING: Ongesuiwerde NiSO4 oplossings word gedurig vervaardig as ŉ produk van die Sherrit gebaseerde mat logingsproses wat lei tot yster en kobalt gekontamineerder oplossings van NiSO4. Om die graad van hierdie oplossings op te gradeer vir die produksie van of NiSO4 kristalle of katode/gepresipiteerde nikkel, moet die yster en kobalt eers verwyder word. Meeste prosesse gebruik of suiwer Cyanex 272 of die natrium sout van Cyanex 272 in ŉ vloeistof-vloeistof ekstraksie siklus om yster en kobalt vanuit versadigde nikkel oplossing te ekstraheer. Hierdie prosesse verg die gebruik van ŉ alkali soos NaOH om die protone te neutraliseer wat geruil word vir die verskillende metaal spesies, aangesien ekstraksie ŉ baie sterk funksie van pH is. Dit het tot gevolg dat natrium tot die oplossing bygevoeg word soos wat yster en kobalt verwyder word. Hierdie tekortkoming kan oorkom word deur Cyanex 272 eers te laai met nikkel deur ŉ porsie van die gesuiwerde nikkel produk te gebruik voor die onsuiwerhede geëkstraheer word. Gedurende die ekstraksie stadium word nikkel dan geruil vir die onsuiwerhede, in plaas van waterstof, en geen NaOH toevoeging is nodig nie. Die gevolg is ŉ suiwer nikkel oplossing. Die geëkstraheerde metaal word herwin vanaf die organies fase deur dit te stroop met ŉ H2SO4 oplossing en die organiese fase kan weer gehersirkuleer word. ŉ Vloeistof-vloeistof ekstraksie proses wat ŉ 80 g/l nikkelsulfaat oplossing van 1 g/l kobalt en 3 g/l yster suiwer, is ontwikkel. Die belangrikste veranderlikes sluit in pH, organies/waterige (O/A) mengingsverhouding, nikkel lading, H2SO4 konsentrasie, Cyanex 272 konsentrasie, verskillende organiese oplosmiddels en temperatuur. Hierdie veranderlikes was ondersoek deur verskeie voorlopige en drie 24 faktoriaal ontwerp enkel-lading eksperimente wat gevolglik die veranderlikes verminder het na pH/NaOH toevoeging en O/A verhouding vir die voorbelading seksie, nikkel lading en O/A verhouding vir die ekstraksie seksie en H2SO4 konsentrasie en A/O verhouding vir die stroping seksie. Die verminderde veranderlikes was verder ondersoek in nog enkel-lading eksperimente, waarvan die data gebruik was om modelle op te stel en ŉ simulasie sigblad in Microsoft Excel te ontwerp van die ekstraksie siklus. Die finale enkel-lading toetse het die kondisies weergegee wat die mees suiwer waterige nikkel produk sal oplewer na ekstraksie, waar kobalt en nikkel selektief van yster gestroop kan word en watter H2SO4 konsentrasie en A/O verhouding nodig is om yster finaal te stroop en die organiese fase te regenereer. Laastens is vier toetse gedoen op ŉ menger-afskeidingstenk opstelling om die betroubaarheid van die simulasie sigblad te toets. Die bedryfstoestande wat voorgestel word vir die vloeistof-vloeistof ekstraksie siklus is om ŉ 20V% Cyanex 272 oplossing in Shellsol D70 as oplosmiddel vooraf te laai met ŉ 80 g/l gesuiwerde nikkel produk oplossing by ŉ O/A verhouding van 25 en ŉ pH van 7 om ŉ nikkel lading van 3.2 g/l vir die ekstraksie seksie te genereer. Hierdie lading by ŉ O/A verhouding van 1.5 produseer ŉ suiwer nikkel waterige oplossing produk (0.05 g/l Co, 0.01 g/l Fe). Vanaf die gegenereerde organiese fase kan die geëkstraheerde nikkel en kobalt selektief gestroop word met 0.1 M H2SO4 by ŉ A/O verhouding van 2.25 gevolg deur ŉ 1 M H2SO4 oplossing by `n A/O verhouding van 0.75 om die oorblywende yster te stroop. Die temperatuur waarby al die stadiums beheer moet word is tussen 40-50°C om fase skeiding te verseker.

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Luo, Haoqun. "The production of food-grade protein isolates from yellow mustard seed by solvent extraction and membrane processng techniques." Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1998. http://www.collectionscanada.ca/obj/s4/f2/dsk1/tape10/PQDD_0004/MQ40911.pdf.

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Bonomi, Élida Castilho 1980. "Extração de pilocarpina e episopiloturina de jaborandi utilizando processos envolvendo solventes supercriticos." [s.n.], 2008. http://repositorio.unicamp.br/jspui/handle/REPOSIP/266131.

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Orientadores: Theo Guenter Kieckbusch, Alvaro Bandeira Antunes de Azevedo, Paulo Mazzafera
Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Quimica
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Resumo: Pilocarpina é um alcalóide encontrado somente nas folhas de jaborandi (Pilocarpus microphyllus), uma espécie vegetal nativa da flora brasileira e empregada principalmente no tratamento de glaucoma e de xerostomia (boca seca). A epiisopiloturina, alcalóide também encontrado no extrato de jaborandi, tem atividade biológica semelhante à pilocarpina, embora atue por mecanismos diferentes. Esta pesquisa teve como objetivo o estudo da aplicabilidade da tecnologia que utiliza fluidos supercríticos na recuperação e purificação destes dois princípios ativos de folhas de jaborandi e de um resíduo industrial semi-sólido gerado na extração de pilocarpina de jaborandi com solventes orgânicos. Os ensaios de extração contemplaram pressões de 200 a 300 bar e temperaturas de 40, 50 e 60ºC, utilizando CO2 puro e CO2 + 10% (em massa) de etanol. Em um estudo complementar investigou-se a influência do acoplamento de uma coluna de adsorção (sílica-gel) em ambiente supercrítico visando purificar os extratos. Os ensaios com CO2 puro indicaram que aumentos de pressão melhoram a capacidade de extração em todas as situações estudadas, sendo esse efeito mais intenso nas extrações de pilocarpina das folhas e de epiisopiloturina da pasta. Aumentos de temperatura favorecem as extrações, exceto nos ensaios realizados a 200 bar, com pilocarpina contida nas folhas, que apresentaram uma tendência inversa, indicativa da proximidade de uma pressão de cruzamento. O CO2 puro mostrou-se pouco eficiente em extrair pilocarpina das folhas. Nas condições avaliadas, a melhor recuperação de pilocarpina ocorreu a 60ºC e na pressão de 300 bar (14,5% das folhas; 84,5% da pasta). O uso de co-solvente (10% etanol) melhorou esse nível de recuperação de pilocarpina e mostrou-se muito mais eficiente na recuperação de epiisopiloturina. Uma contaminação do extrato com clorofila foi observada no processamento das folhas de jaborandi com CO2 puro e que se intensifica com o uso de etanol, prejudicando a pureza dos mesmos. A sílica-gel mostrou ter maior afinidade pela clorofila do que com os alcalóides. No processo extração/adsorção, a clorofila é completamente adsorvida na sílica, deslocando as moléculas de pilocarpina e de epiisopiloturina, indicativo de que esta pode ser uma alternativa promissora para a produção de um extrato de alta qualidade. Os ensaios de extração/adsorção com a pasta residual indicaram que a sílica-gel não é capaz de separar a pilocarpina da epiisopiloturina.
Abstract: Pilocarpine is an alkaloid found only in jaborandi leaves (Pilocarpus microphyllus), a native tree of Brazil, and is widely used in the treatment of glaucoma and xerostomia (dry mouth). Epiisopiloturine, another alkaloid also found in jaborandi has a similar biological activity, acting by different mechanisms. This research evaluated the applicability of the technology that uses supercritical fluid (SCF) in the recovery of these two active compounds from jaborandi leaves and from an industrial pastelike residue produced during extraction of pilocarpine with organic solvents. The SCF extractions runs used pure CO2 and CO2 + 10% (m/m) ethanol at pressures of 200 and 300 bar and temperatures of 40, 50 and 60ºC. In an additional study, a silica gel adsorption stage was coupled to the system in an attempt to purify the extracts. Results using pure CO2 indicate that increases in pressure increase the extraction capacity in all situations studied, more intensively the pilocarpine extraction from the leaves and epiisopiloturine from the paste. Higher temperatures improved the extraction rates, except for pilocarpine extractions from the leaves, at 200 bar, when a reverse trend was found, signalizing the proximity of a crossing pressure. Pure CO2 showed poor effectiveness in extracting pilocarpine from the leaves. At the conditions evaluated, the highest recovery found for pilocarpine was at 60°C and 300 bar (14.5% from the leaves; 64.5% from the paste). The addition of a co-solvent (10% ethanol) boosted the pilocarpine recovery level, and was even more effective in the recovery of epiisopiloturine. The pure CO2 leaves extracts were contaminated with chlorophyll, a condition aggravated when CO2 with ethanol was used. Silica showed higher affinity for chlorophyll than for the alkaloids. In the extraction/adsorption coupled process, all chlorophyll was adsorbed on silica, displacing the pilocarpine and epiisopiloturine molecules, and suggesting a suitable alternative for the production of high quality extracts. The extraction/adsorption runs using the paste indicated that silica was unable to separate pilocarpine from epiisopiloturine.
Mestrado
Engenharia de Processos
Mestre em Engenharia Química

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Santos, Kátia Andressa. "Estudo dos processos de extração do óleo de candeia (Eremanthus erythropappus) com fluidos pressurizados e solvente assistido por ultrassom." Universidade Estadual do Oeste do Paraná, 2018. http://tede.unioeste.br/handle/tede/3579.

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Candeia (Eremanthus erythropappus) is a native species of the Brazilian Atlantic forest from which an essential oil with high concentration of sesquiterpene α-bisabolol is extracted. α-Bisabolol is an active principle of important application in the cosmetic and pharmaceutical industries due to its anti-inflammatory, antispasmodic, sedative, antiallergic, anti-irritant, cicatrizant and vermifugal properties. Steam distillation is the most common method used to obtain this oil, with requires long periods of time extraction besides the degradation of thermosensitive compounds. Within this context, the aim of this study was to evaluate the quality of the candeia wood oils obtained by non-conventional methods of extraction (supercritical technology by using carbon dioxide and cosolvents, pressurized liquid and ultrasound-assisted extraction), in terms of oil yield, bisabolol content and antioxidant activity. In addition, the oil re-extraction from the industrial residue was also evaluated. The extractions were carried out with CO2 at temperatures of 40, 55 and 70 oC and pressures of 160, 200 and 240 bar, with a solvent mass flow rate of 1.96 x 10−3 kg min−1 and 120 min of total extraction. The highest extraction yield obtained was 1.42 wt% for the candeia wood and 0.41 wt% for the residue, both at 70 oC and 240 bar, and this condition was selected to perform the extractions using cosolvents. Ethanol and ethyl acetate were added to supercritical CO2 at concentrations of 1, 3 and 5 % (v/v), obtaining up to 2.35 wt% of yield. The Soxhlet (360 min) and pressurized liquid (40, 55 and 70 oC; 100 bar and 20 min) extractions showed the affinity of the candeia compounds for polar solvents and the positive effect of the temperature on the yield, which varied from 0.53 to 7.23 wt%. A Box-Benhken design was employed to evaluate the effect of the variables temperature (40, 50 and 60 oC), n-hexane volume to wood mass (10, 15 and 20 mL g-1) and nominal power (150, 300 and 450 W) on the yield of ultrasound-assisted extractions, obtaining in 7 minutes of extraction, up to 83% of the yield obtained in the conventional technique in Soxhlet (1.57 wt%), with a solvent volume 2.5 times smaller. The major compounds identified in the candeia oil were the sesquiterpenes α-bisabolol, eremanthin and costunolide, and the α-bisabolol content in the oil is favored by the lowest CO2 density, with 74.45 % being obtained for the candeia wood and 50.62 % for the residue, in both cases in oil extracted at 70 oC and 160 bar. The addition of ethanol and ethyl acetate cosolvents to CO2 increased the α-bisabolol yield by 41 %. Also, the cosolvents increased the amount of total phenolic content in the oil, and consequently, its antioxidant capacity. The oil fractionation by column chromatography was efficient for α-bisabolol isolation. However, unlike the candeia wood oil, this compound was not effective in inhibiting the Staphylococcus aureus growth. In relation to the supercritical extractions, the Sovová mathematical model presented a good adjustment to the experimental data for all the conditions used.
A candeia (Eremanthus erythropappus) é uma árvore nativa da Mata Atlântica da qual se extrai um óleo essencial com elevada concentração do sesquiterpeno α-bisabolol, princípio ativo de grande aplicação nas indústrias de cosméticos e farmacêutica devido às suas propriedades anti-inflamatória, antiespasmódica, sedativa, antialérgica, anti-irritante, cicatrizante e vermífuga. A obtenção deste óleo em escala industrial é realizada pelo processo de destilação por arraste a vapor, com elevado tempo de extração, além da degradação de compostos termossensíveis. Neste contexto, o presente trabalho tem como objetivo avaliar a qualidade dos óleos da madeira de candeia, obtidos por métodos não convencionais de extração (tecnologia supercrítica com dióxido de carbono e cossolventes, líquidos pressurizados e solvente assistido por ultrassom), em termos de rendimento, teor de α-bisabolol e atividade antioxidante. Ainda, avaliar a re-extração do óleo do resíduo industrial. As extrações foram realizadas com CO2 nas temperaturas de 40, 55 e 70 oC e pressões de 160, 200 e 240 bar, com vazão mássica de solvente de 1,96 x 10-3 kg min-1 e tempo total de 120 minutos. O maior rendimento obtido para o óleo da candeia nas extrações supercríticas foi de 1,42 % e de 0,41 % para o resíduo, ambos em 70 oC e 240 bar, condição selecionada para os experimentos com cossolventes. Os solventes etanol e acetato de etila foram utilizados nas concentrações de 1, 3 e 5 % (v/v) junto ao CO2, proporcionando rendimentos de até 2,35 %. As extrações Soxhlet (360 min) e com líquidos pressurizados (40, 55 e 70 oC; 100 bar e 20 min) evidenciaram a afinidade dos compostos por solventes polares e o efeito positivo da temperatura sobre o rendimento, de 0,53 a 7,23 %. Um planejamento Box-Behnken foi empregado para avaliar efeitos da temperatura (40, 50 e 60 oC), razão volume de n-hexano/massa de madeira (10, 15 e 20 mL g-1) e potência ultrassônica nominal do equipamento (150, 300 e 450 W) sobre rendimento em óleo, obtendo-se, em 7 minutos de extração, até 83 % do rendimento obtido na técnica convencional em Soxhlet (1,57 %), com volume de solvente 2,5 vezes menor. Os compostos majoritários identificados no óleo da candeia foram os sesquiterpenos α-bisabolol, eremantina e costunolida, e o conteúdo do α-bisabolol no óleo foi favorecido pela menor densidade do CO2 supercrítico, sendo de até 74,5 % para a madeira de candeia e 50,6 % para o resíduo, ambos extraídos na condição de 70 oC e 160 bar. A adição dos cossolventes etanol e acetato de etila ao CO2 elevou o rendimento de α-bisabolol em até 41 %. Também aumentaram a quantidade de fenólicos totais no óleo e, consequentemente, sua capacidade antioxidante. O fracionamento do óleo por cromatografia em coluna foi eficiente para o isolamento do α-bisabolol. No entanto, diferentemente do óleo da madeira de candeia, este composto não foi efetivo na inibição do crescimento de Staphylococcus aureus. Em relação às cinéticas das extrações supercríticas, o modelo matemático de Sovová se ajustou aos dados experimentais em todas as condições utilizadas.

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Ben, Amor Bouthaina. "Maîtrise de l'aptitude technologique de la matière végétale dans les opérations d'extraction de principes actifs : texturation par détente instantanée contrôlée (DIC)." Phd thesis, Université de La Rochelle, 2008. http://tel.archives-ouvertes.fr/tel-00399131.

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Le présent travail de thèse porte sur l‘étude de l‘effet de la texturation par Détente Instantanée Contrôlée (DIC) sur l‘opération d‘extraction solide liquide d‘oligosaccharides à partir des graines de Tephrosia purpurea et d‘anthocyanes à partir de calices de Roselle (Hibiscus sabdariffa) en vue d‘améliorer la cinétique et le rendement d‘extraction. Une analyse fondamentale a prouvé l‘importance de la diffusion du solvant dans la matrice solide et de l‘extrait dans le solvant, en tant que principal processus limitant. L‘expansion de la structure solide a donc été identifiée comme principale action devant mener à l‘intensification de l‘opération. L‘effet des paramètres opératoires de la DIC (pression de vapeur et temps de traitement thermique) a été quantifié. L‘étude a montré la capacité du traitement par DIC d‘intensifier l‘opération en termes de cinétique et de rendement d‘extraction dans les deux cas du cicéritol et du stachyose à partir des graines de Tephrosia purpurea et d‘anthocyanes à partir de calices de Roselle (Hibiscus sabdariffa). Dans le cas des oligosaccharides, le temps d'extraction a été réduit à une heure au lieu de 4h. Le rendement a été amélioré d'un facteur de 150%. Concernant les anthocyanes, le temps d‘extraction a été réduit à 3 minutes au lieu de 10 minutes et le rendement a été amélioré d‘un facteur de 120%. Une étude phénoménologique a permis de déterminer la valeur de la diffusivité d‘extraction de ces différentes molécules dans la matière première et dans les matériaux différemment traités par DIC. Les effets de la température d‘extraction et du solvant ont également été étudiés dans le cas de l‘extraction des oligosaccharides.

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Addo, Douglas Kweku. "OPERATION AND PROCESS CONTROL DEVELOPMENT FOR A PILOT-SCALE LEACHING AND SOLVENT EXTRACTION CIRCUIT RECOVERING RARE EARTH ELEMENTS FROM COAL-BASED SOURCES." UKnowledge, 2019. https://uknowledge.uky.edu/mng_etds/50.

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The US Department of Energy in 2010 has identified several rare earth elements as critical materials to enable clean technologies. As part of ongoing research in REEs (rare earth elements) recovery from coal sources, the University of Kentucky has designed, developed and is demonstrating a ¼ ton/hour pilot-scale processing plant to produce high-grade REEs from coal sources. Due to the need to control critical variables (e.g. pH, tank level, etc.), process control is required. To ensure adequate process control, a study was conducted on leaching and solvent extraction control to evaluate the potential of achieving low-cost REE recovery in addition to developing a process control PLC system. The overall operational design and utilization of Six Sigma methodologies is discussed. Further, the application of the controls design, both procedural and electronic for the control of process variables such as pH is discussed. Variations in output parameters were quantified as a function of time. Data trends show that the mean process variable was maintained within prescribed limits. Future work for the utilization of data analysis and integration for data-based decision-making will be discussed.

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Ager, Patrick. "Recycle of complexing reagents during mechanical pulping." Thesis, McGill University, 2003. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=82813.

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The stability of hydrogen peroxide (H2O2) is a critical factor for the brightening of mechanical pulps. Inorganic ions, including Fe, Mn and Cu catalytically decompose H2O2. These troublesome metals promote the rapid transformation of H2O2 to nonselective hydroxyl radicals that degrade the cellulose fibres and decrease yields.
The interaction of aqueous metal•complexes with magnesium metal (Mg°) or bimetallic mixtures of magnesium with either palladium (Pd°/Mg°) or silver (Ag°/Mg°) were optimized to remove metals (Mn, Cu and Fe) from solution with concomitant release of the complexing reagent. The analyte metals were removed by both cementation on the surfaces of the excess Mg° and by precipitation as hydroxides. Overall, the reactions were rapid (3 or 10 min) and very efficient. The accelerators (Ag or Pd) were deposited on the surfaces of the Mg°. In a separate study, the excess of Mg° could be reused to mediate more metals removal without apparent loss of reactivity. Among the other iminodiacetate analogs (CDTA, MEDTA, EGTA, HEDTA, DPTA and MTBE), the EGTA and HEDTA proved to be possible substitutes for both efficient metal removal of Mn, Cu and Fe from solution and efficient release of chelating reagent. The measurement of particle size, performed by laser granulometry, demonstrated that smaller particles of precipitate were generated from metal-EDTA complexes by reaction with NaOH than by reaction with Pd°/Mg° bimetallic mixture. If the suspensions of particles were analyzed in the absence of ultrasound, the particles became aggregated into large flocs (up to 150 mum3 ). The reactivity of the bimetallic mixtures was exploited to remove Cu, Mn, Fe, Zn and Al that had been initially chelated with EDTA or DTPA from a thermomechanical pulp (TMP). After 15 min, the metals had been removed efficiently with the bimetallic mixtures. The EDTA released from the TMP filtrate could be recycled efficiently for a total of three cycles. On the other hand, the DTPA was not released as efficiently. Measurements of turbidity and chemical oxygen demand (COD) indicated no appreciable difference between the pulp samples with either chelating reagent. Residual H2O2 and ISO brightness measurements indicated no apparent differences among pulps that had been treated wi

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Klein, Elissandro Jair. "Obtenção de compostos bioativos de folhas de uvaia (Eugenia pyriformis Cambess.) utilizando CO2 supercrítico e extração com solvente assistida por ultrassom." Universidade Estadual do Oeste do Paraná, 2016. http://tede.unioeste.br/handle/tede/3729.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES
Eugenia pyriformis Cambess. (Uvaia), typical of the Atlantic Forest belongs to the Myrtaceae family, the same family of cherry, jabuticaba and other plants, currently studied due to their antioxidant, antimicrobial and medicinal properties. The interest in bioactive compounds obtained from natural sources has led to an increase in researches aiming to find these compounds in plant extracts. The extractions using conventional methods generally have some drawbacks, and an interesting alternative has been the use of non-conventional extraction technologies, such as the supercritical fluid and the ultrasound-assisted extraction. This work aims to study unconventional methods of obtaining uvaia extracts in order to obtain extracts rich in bioactive compounds. Factors such as the influence of type of extraction (supercritical fluid and ultrasound) and the used conditions on the yield and composition were evaluated. The results were compared to those obtained using the extraction by maceration, a conventional extraction method. After drying and milling the uvaia leaves, the plant material was subjected to extraction with the supercritical CO2 solvent under different conditions of temperature (40, 50 and 60 °C) and pressure (100, 150 and 200 bar), with a fixed flow of 2.0 kg min-1. In the ultrasound-assisted extraction, the effects of temperature (40, 50 and 60 °C), power (150, 250 and 350 W) and ratio between the mass of leaves and the volume of solvent (1:10, 1:15 and 1:20) were evaluated. The extracts obtained were chemically characterized by GC-MS giving β-amyrin (53.72 % for SFE and 71.25 % for UAE) and α-amyrin (24.63 % for SFE and 22.69 % for UAE) as main compounds. In the supercritical extraction, the pressure and the interaction between pressure and temperature showed statistically significant effects on the yield, with the best result being achieved at 200 bar and 60 °C, reaching 1.69%. The data obtained from the supercritical fluid extraction were used to adjust the extraction curves simulated by using two empirical models available in the literature. The tested models adjusted well to the experimental data and the analysis of the estimated parameters allowed to define which model best describes the kinetics of each experimental condition. For the ultrasound-assisted extraction, the best yield result found in the determination of the kinetics was 1.81% in 40 minutes, although in the experimental design a 3 minute time extraction was used due to the better characteristics showed by the extracts at this time. The best result obtained in experimental design with ultrasound was 1.79% provided 30% power, 60 °C and mas/solvent ratio 1:20. Statistical analysis of the experimental design of the ultrasound-assisted extraction indicated significant effects from the variables temperature, mass/solvent ratio and the interaction between power and mass/solvent ratio. The best results for amyrin content by extract weight was found for supercritical extraction, with 97.43%. The ultrasound-assisted extraction showed the best amyrin amount per mass of leaves, 12.13 g of the mixture of isomers per kg of dry leaf.
Eugenia pyriformis Cambess. (Uvaia), típica da Mata Atlântica pertence à família Myrtaceae, mesma família da pitanga, jabuticaba e outras plantas, atualmente estudadas devido às suas propriedades antioxidantes, antimicrobianas e medicinais. O interesse por compostos bioativos obtidos de fontes naturais tem levado ao aumento no número de pesquisas que visam encontrar esses compostos em extratos de plantas. As extrações que utilizam os métodos convencionais geralmente apresentam inconvenientes, e uma alternativa interessante tem sido a utilização de tecnologias não convencionais de extração, como a extração utilizando fluidos supercríticos e a extração assistida por ultrassom. O presente trabalho tem como objetivo estudar métodos não convencionais de obtenção de extratos de uvaia visando obter-se extratos ricos em compostos bioativos. Foram avaliados fatores como influência do tipo de extração (fluido supercrítico e ultrassom) e das condições utilizadas no rendimento e na composição. Os resultados foram comparados com os obtidos utilizando a extração por maceração, um método convencional de extração. Após secagem e moagem das folhas de uvaia, o material vegetal foi submetido à extração com o solvente CO2 supercrítico sob diferentes condições de temperatura (40, 50 e 60 oC) e de pressão (100,150 e 200 bar), com vazão fixa de 2,0x10-3 kg min-1. Na extração assistida por ultrassom, foram avaliados os efeitos da temperatura (40, 50 e 60 oC), da potência (150, 250 e 350 W) e razão entre massa de folhas e volume de solvente (1:10, 1:15 e 1:20). Os extratos obtidos foram caracterizados quimicamente por CG-EM apresentando com principais compostos β-amirina (53,72 % para EFS e 71,25 % para EAU) e α-amirina (24,63 % para EFS e 22,69 % para EAU). Na extração supercrítica, a pressão e a interação entre pressão e temperatura apresentaram efeitos estatisticamente significativos em relação ao rendimento, sendo que o melhor resultado foi encontrado com 200 bar e 60 oC, obtendo-se 1,69 %. Os dados obtidos na extração com fluido supercrítico foram utilizados para ajustar as curvas de extração simuladas utilizando dois modelos empíricos disponíveis na literatura. Os modelos testados ajustaram-se de forma satisfatória aos dados experimentais e a análise dos parâmetros estimados permitiu definir qual dos modelos melhor se ajustou à cinética de cada condição experimental. Para a extração assistida por ultrassom o melhor resultado de rendimento encontrado na determinação da cinética foi 1,81 % com 40 minutos, porém no planejamento experimental foi utilizado um tempo de extração de 3 minutos pois com esse tempo os extratos apresentavam melhores características, sendo portanto o melhor resultado obtido igual a 1,79 % na condição de 30 % de potência, 60 oC e razão massa/solvente de 1:20. A análise estatística do planejamento experimental da extração assistida por ultrassom indicou efeitos significativos das variáveis temperatura, razão massa/solvente e a interação entre potência e razão massa/solvente. Os melhores resultados de teor de amirina por massa de extrato foi encontrada para a extração supercrítica, com 97,43 %. A extração assistida por ultrassom apresentou a melhor quantidade de amirina por massa de folha, 12,13 g da mistura de isômeros por kg de folha seca.

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Obón, Estrada Eleonora. "Towards the recovery of rare earth elements from end-of-life products : hydrometallurgical routes and mathematical modelling of extraction systems." Doctoral thesis, Universitat Politècnica de Catalunya, 2019. http://hdl.handle.net/10803/669262.

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The rare earth elements (REEs) are essential ingredients for the development of modern industry and the transition to a more sustainable economy model. The unique physicochemical features of these elements, such as their magnetism and optical properties, are greatly expanding their application. They have become key elements for the manufacture of many ordinary consumer goods like hybrid cars, fluorescent lamps or electronic devices like mobile phones or tablets. The growing popularity of the rare earth elements derivatives is leading to an increase in the global demand and the price of these elements. Unfortunately, the current availability of these resources is limited due to three main factors: their heterogeneous geological location, their low concentration in the ores, and the environmental issues related with their mining. All these disadvantages concerning the supply of the rare earth elements have led to the study of new techniques to obtain them, such as the recycling of end-of-life products. Recycling of REEs arises as a new secondary source of supply of REEs, especially in Europe where large amounts of technological waste are generated every year. Currently, the recycling of rare earth elements represents less than 1% of the global supply. Nevertheless, some studies in the literature assume that by 2050 the recovery rate of REEs will be 90% for wind turbines, 70% for electrical vehicles and 40% for the rest of derivative products. The research presented in this thesis relies on experimental investigation of new hydrometallurgical routes, the majority of them involving the use of ionic liquids, which could eventually be applied for the recovery of rare earth elements from end-of-life products. Matemathical modelling of the reported extraction systems has been carried out in order to provide a computational instrument that can be easily tailored for prediction of other collecting processes requiring minor adjustments.
Les terres rares son ingredients essencials per al desenvolupament de la indústria moderna i la transició cap a un model econòmic més sostenible. Les seves característiques físico-químiques úniques, com el seu magnetisme i propietats òptiques, han precipitat un increment accelerat en l’aplicació d’aquests elements. Les terres rares s’han convertit en elements clau per a la fabricació de molts articles d’ús diari com per exemple, cotxes elèctrics i dispositius electrònics com telèfons mòbils i tabletes. La creixent popularitat dels productes que contenen aquests metalls està provocant un escalat en la demanda global i el preu de les terres rares. Desafortunadament, en l’actualitat, la disponibilitat d’aquests recursos a la natura és limitada degut bàsicament a tres factors: heterogènia localització geològica, baixa concentració als minerals que els contenen i inconvenients mediambientals relacionats amb la mineria. Els inconvenients relacionats amb el subministrament de les terres rares a nivell mundial han propiciat l’estudi de noves tècniques per a la obtenció d’aquests elements mitjançant el reciclatge de productes que els contenen. El reciclatge sorgeix com una font secundària alternativa a la mineria per tal d’assegurar el provisionament de terres rares especialment a Europa, on generem grans quantitats de residus tecnològics cada any. Actualment, la taxa de reciclatge de terres rares se situa per sota l'1% del subministrament global. No obstant, alguns estudis publicats en la literatura assumeixen que l’any 2050, la taxa de recuperació haurà augmentat considerablement, de manera que es reciclarà fins a un 90% de les terres rares provinents d’aerogeneradors, 70% de vehicles elèctrics i 40% de la resta de productes que contenen aquests metalls. La recerca presentada en aquesta tesi es basa, principalment, en la investigació de noves rutes hidrometal·lúrgies, la majoria d’elles utilitzant líquids iònics, que puguin ser implementades en processos de recuperació de terres rares a partir de residus tecnològics. D’altra banda, s’han elaborat models matemàtics dels sistemes d’extracció reportats que pretenen convertir-se en una eina computacional, fàcilment adaptable, per a la predicció del comportament d’extracció en d’altres processos de recuperació amb diferents condicions experimentals.

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Minier, Michel. "Fermentation acetonobutylique par couplage a des procedes membranaires et fermentation extractive." Toulouse 3, 1987. http://www.theses.fr/1987TOU30290.

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29

Cesari, Laëtitia. "Extraction de composés phénoliques à partir d’une bio-huile de lignine." Thesis, Université de Lorraine, 2017. http://www.theses.fr/2017LORR0148/document.

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La biomasse ligno-cellulosique est principalement constituée de cellulose, d’hémicellulose et de lignine. Par conversion thermochimique, la lignine se transforme en bio-huile riche en composés phénoliques. Ces composés phénoliques sont généralement récupérés à l’aide de plusieurs étapes d‘extractions liquide-liquide consécutives impliquant des solvants aqueux et organiques. À l’aide d’une approche multi-échelle, nous avons étudié, la faisabilité et l’efficacité d’un liquide ionique, la [Choline][NTf2], pour l’extraction liquide-liquide de ces composés. En effet, l’utilisation de ce solvant permettrait d’améliorer l’efficacité d’extraction, tout en diminuant la toxicité et les coûts liés à l’utilisation de solvants organiques classiques. Des calculs quantiques ont été effectués afin de mieux comprendre les interactions régissant les systèmes clés de ces extractions. Les structures des composés phénoliques dans leur état isolé ou en présence de solvant montrent que les conformations sont stabilisées par la présence de liaisons hydrogène. De plus, la détermination des énergies d’interaction indique que la [Choline][NTf2] est efficace pour l’extraction de composés phénoliques présents en solution aqueuse. Par ailleurs, la détermination des diagrammes de phases des systèmes binaires {eau-composé + phénolique} et des systèmes ternaires {eau + composé phénolique + [Choline][NTf2]} montre que l’extraction des composés est également possible à une échelle macroscopique. Les paramètres NRTL issus de ces expériences ont permis de simuler l’extraction de trois composés phénoliques majoritairement présents dans les bio-huiles, i.e. le phénol, le guaiacol et le syringol, et ce, à moindre coût. Enfin, l’extraction de ces composés à partir d’une bio-huile obtenue par pyrolyse rapide de lignine a également été particulièrement efficace avec le liquide ionique [Choline][NTf2]. De ce fait, cette étude multi-échelle a permis de montrer que la [Choline][NTf2] est un excellent solvant pour la récupération des composés phénoliques. Enfin, l’étude des propriétés anti-oxydantes témoigne de la valeur ajoutée de ces composés, notamment à travers leur pouvoir réducteur et leur propriété anti-radicalaire
The lignocellulosic biomass is mostly composed of cellulose, hemicellulose and lignin. Upon thermal conversion of lignin, a bio-oil rich in phenolic compounds is obtained. These latter are then generally recovered through several liquid-liquid extraction involving aqueous and organic solvents. In this work we investigated, by a multi-scale study, the feasibility and the efficiency of the ionic liquid [Choline][NTf2] for the extraction of these phenolic compounds by liquid-liquid extraction. Indeed, such a solvent could improve the extraction efficiency and at the same time, reduce the toxicity and the cost of the classic organic solvents. Quantum calculations were performed in order to better understand the interaction governing the key systems of these extractions. The structures of the phenolic compounds in their isolated forms and in contact with solvents show that the conformations are stabilized by the presence of hydrogen bonds. More, the determination of the interaction energies indicates that the [Choline][NTf2] ionic liquid is efficient for the extraction of phenolic compounds present in aqueous solution. Furthermore, the study of phase diagrams of binary systems {water-phenolic compound} and ternary systems {water-phenolic compound-[Choline][NTf2]} show that the extraction of these compounds is also possible at a macroscopic scale. Then, the NRTL parameters coming from these experiments allowed the simulation of the extraction of three compounds mostly present in the bio-oils, namely phenol, guaiacol and syringol, as so at low cost. Finally, the extraction of these compounds from bio-oil obtained from lignin fast pyrolysis was also particularly efficient with the [Choline][NTf2] ionic liquid. Therefore, this multi-scale study demonstrated that [Choline][NTf2] is an excellent solvent for the recovery of phenolic compounds. Lastly, the study of the antioxidant properties testify the added-value of these compounds, especially through their reducing power and their radical scavenging capacity

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Christen, Pierre. "Faisabilite d'un procede a membrane liquide pour l'extraction continue de l'ethanol produit par fermentation." Paris, ENMP, 1987. http://www.theses.fr/1987ENMP0055.

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Une membrane liquide composee d'un support poreux hydrophobe impregne d'un solvant organique a ete mise au point; l'isotridecanol s'est avere etre biocompatible, impermeable aux sels et au glucose et autorise un flux d'ethanol important (35 g/h. M**(2)). Cette membrane liquide mise en oeuvre avec une phase receptrice aqueuse a permis, par l'extraction de l'ethanol inhibiteur, une detoxification significative d'un mout de fermentation en activite: amelioration de la viabilite des levures et de productivite du fermenteur d'un facteur 2,5. En outre, ce procede d'extraction a permis de mettre en evidence l'activite inhibitrice de metabolites secondaires. Une etape supplementaire de concentration en ligne de l'ethanol extrait peut etre realisee en utilisant le procede a membrane liquide avec une phase receptrice gazeuse et un piege a froid. Enfin, une modelisation mathematique des phenomenes de transfert d'ethanol a travers une membrane liquide a permis de mieux cerner les resistances au transfert et a montre l'importance de parametres lies au support (epaisseur, porosite, tortuosite, des pores) et lies au solvant (coefficient de partage et diffusivite)

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31

SENEDA, JOSE A. "Separação e recuperação de chumbo-208 dos resíduos de tório terras raras gerados na unidade piloto de purificação de nitrato de tório." reponame:Repositório Institucional do IPEN, 2006. http://repositorio.ipen.br:8080/xmlui/handle/123456789/11424.

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Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

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32

Marin, Gallego Mylene. "Valorisation chimique des condensats issus de la torréfaction de biomasses : modélisation thermodynamique, conception et analyse des procédés." Thesis, Toulouse, INPT, 2015. http://www.theses.fr/2015INPT0131.

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La biomasse lignocellulosique est considérée comme une ressource de carbone renouvelable possédant un grand potentiel pour la une valorisation énergétique et chimique. La torréfaction de la biomasse sèche (de type bois) est un procédé de transformation thermique s’effectuant à des températures comprises entre 200°C et 300°C, et un temps de séjour compris entre quelques minutes et plusieurs heures, opérant sous pression atmosphérique et en défaut d’air. Le produit principal de la torréfaction est un combustible solide hydrophobe et stable. Cette opération génère des coproduits gazeux à haute température qui sont habituellement considérés comme des effluents pénalisants, apportant au mieux un appoint d’énergie pour le procédé. Pourtant, de nombreux constituants présents dans les condensats – récupérés par condensation des coproduits de torréfaction – pourraient être valorisés comme produits chimiques bio-sourcés. L'objectif de la thèse est de proposer un procédé de séparation-purification pour les composés condensables présents dans ces effluents gazeux. Ces condensats constituent une phase majoritairement aqueuse, contenant plus de 150 espèces organiques identifiées. Les espèces minoritaires sont présentes dans des proportions variables suivant le bois torréfié. Enfin il s’agit d’un mélange réactif et thermiquement instable, où différents équilibres chimiques sont présents. Une analyse des caractéristiques physico-chimiques des condensats a permis de proposer un milieu modèle limité à une dizaine de composés. Un modèle représentatif du comportement thermodynamique de ce mélange réactif à large spectre de masse moléculaire a été sélectionné et les paramètres d’interaction binaire identifiés. Des données expérimentales d’équilibres liquide-vapeur ont été acquises pour valider en partie ce modèle. Les composés cibles et les objectifs du procédé de valorisation ont été choisis et plusieurs stratégies de valorisation ont été élaborées et simulées sous Prosim+ sur la base de la modélisation thermodynamique. Cette étude a permis d’évaluer ces différentes stratégies en termes d’efficacité énergétique et de pureté des produits finaux pour une potentielle mise en place à l’échelle industrielle de cette filière
Lignocellulosic biomass is considered as a renewable carbon resource with great potential for the energy and chemical recovery. Torrefaction is a thermal process carried out at temperatures below 300°C, under inert atmosphere, at atmospheric pressure, and with residence times for the solid biomass ranging from few minutes to several hours. Torrefied wood is a solid product constituted by more than 70% of the initial mass with properties close to those of coal. The 30% remaining part is a gaseous effluent, composed of about one third of non-condensable gases – carbon monoxide and carbon dioxide – and two thirds of condensable species. Currently, torrefied wood is the main product of interest and is usually transformed into energetic gases by the gasification process or directly used as coal for combustion. Conversely, gaseous by-products are considered at present time as a waste and in the best case are burned to provide energy to the process. Yet, the recovery and valorization of the condensable fraction as bio-sourced chemicals is worth considering. The aim of the thesis is to propose a separation-purification process for condensable chemicals of the waste gas. This condensable fraction is a predominantly aqueous phase, containing more than 150 identified organic species. Minority species are present in varying proportions depending on torrefied wood. Finally, it is a reactive and thermally unstable mixture, where different chemical equilibria are present. An analysis of the physicochemical characteristics of the condensable fraction allowed selecting a limited number of compounds to model the mixture. A representative model of the thermodynamic behavior of the reactive mixture has been selected and the binary interaction parameters identified. Experimental vapor-liquid equilibria data were acquired in part to validate this model. The target compounds and objectives of the recovery process were selected and several development strategies were developed and simulated in ProSim+ on the basis of thermodynamic modeling. This study assessed these different strategies in terms of energy efficiency and purity of the products for potential implementation on an industrial scale of this sector

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33

Nimet, Graziane. "Avaliação dos solventes dióxido de carbono supercrítico e propano subcrítico na extração do óleo de girassol." Universidade Estadual do Oeste do Parana, 2009. http://tede.unioeste.br:8080/tede/handle/tede/1882.

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The extraction of oil from greasy seeds is traditionally based in the use of organic solvents. Currently the most used method is the process of extraction by n-hexane. Aiming the obtainment of vegetable oil with higher quality using clean technologies with reduction of oil contamination through solvent and minimizing the damage to the environment is that the technology with fluid pressurized has become one alternative viable to extraction. In this context, the current work has the objective to compare the extraction of the oil in sunflower seeds using the carbon dioxide as solvent in supercritical conditions, the propane in subcritical conditions and the n-hexane. At the beginning, the sunflower seeds were characterized, then went by drying process, crush and sifting and, finally through the extraction process. The experiments were led in temperatures of 40, 50, and 60 °C and pressures of 19, 22 e 25 MPa to carbon dioxide, and temperatures of 30, 45 e 60 ºC and pressures of 8, 10, and 12 MPa to propane. It was considered the effect of the temperature and pressure in the reason of the weight the extracted sunflower oil per weight of solvent used to the different experimental conditions, using a factorial planning 22 with 3 repetitions in the central point. The samples of oil extracted were subordinated to quantification analysis of fatty acids, concentrated of vitamin E (α-tocopherol) and stability oxidative. The pie was analyzed as for its protein content. From the experimental data of the extractions kinetics were tasted the Mathematical models of second order and the Sovová. The results showed that extraction with propane subcritical presented higher rate of extraction when compared to carbon dioxide and to n-hexane, indicating that the propane is a solvent more appropriate to extraction of sunflower oil than the carbon dioxide. The sunflower oil obtained in different experimental conditions didn t present alterations as for the content of fatty acids, however, it was noticed difference in the concentration of vitamin E (α-tocopherol). The samples of oils extracted as in supercritical conditions with carbon dioxide as in subcritical conditions using propane presented better oxidative stability, indicated by the induction time of oxidation than the sample extracted with n-hexane. The pies presented protein contents close independent to the solvent used in the extraction of sunflower oil. The Mathematical modeling of second order and the Sovová model were adapted properly to the experimental data of both solvents.
A extração de óleos de sementes oleaginosas é tradicionalmente baseada no uso de solventes orgânicos. Atualmente o método mais utilizado é o processo de extração por n-hexano. Visando a obtenção de óleos vegetais com maior qualidade utilizando tecnologias limpas com redução de contaminação do óleo pelo solvente e minimizando os danos ao meio ambiente é que a tecnologia com fluidos pressurizados tem se tornado uma alternativa viável de extração. Neste contexto, o presente trabalho teve como objetivo comparar a extração do óleo de sementes de girassol utilizando como solventes o dióxido de carbono em condições supercríticas, o propano em condições subcríticas e o n-hexano. Inicialmente as sementes de girassol foram caracterizadas, então passaram por processo de secagem, moagem e peneiramento e finalmente pelo processo de extração. Os experimentos foram conduzidos em temperaturas de 40, 50 e 60 ºC e pressões de 19, 22 e 25 MPa para o dióxido de carbono, e temperaturas de 30, 45 e 60 ºC e pressões de 8, 10 e 12 MPa para propano. Avaliou-se o efeito da temperatura e pressão na razão de massa de óleo extraída por massa de solvente utilizado para as diferentes condições experimentais, usando um planejamento fatorial 22 com 3 repetições no ponto central. As amostras de óleo extraídas foram submetidas a análises de quantificação de ácidos graxos, concentração de vitamina E (α-tocoferol) e estabilidade oxidativa. A torta foi analisada quanto ao seu teor protéico. A partir dos dados experimentais das cinéticas de extrações foram testados os modelos matemáticos de segunda ordem e de Sovová. Os resultados mostraram que extrações com propano subcrítico apresentaram maior taxa de extração quando comparado ao dióxido de carbono e ao n-hexano, indicando que o propano é um solvente mais apropriado para extração do óleo de girassol do que o dióxido de carbono. O óleo de girassol obtido nas diferentes condições experimentais não apresentou alterações quanto ao teor de ácidos graxos, porém, observou-se diferença na concentração de vitamina E (α-tocoferol). As amostras de óleo extraído tanto em condições supercríticas com dióxido de carbono, quanto em condições subcríticas utilizando propano apresentaram melhor estabilidade oxidativa, indicada pelo tempo de indução da oxidação, do que a amostra extraída com n-hexano. As tortas apresentaram teores protéicos próximos independente do solvente empregado na extração do óleo de girassol. O modelo matemático de segunda ordem e o modelo de Sovová ajustaram-se adequadamente aos dados experimentais de ambos os solventes.

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Silva, Simone Braga da. "Estudo da extração do óleo de pitanga (Eugenia uniflora L.) vermelha e roxa empregando os solventes CO2 e n - propano em altas pressões." Universidade Estadual do Oeste do Parana, 2012. http://tede.unioeste.br:8080/tede/handle/tede/1908.

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From Surinam cherry s leaves (Eugenia uniflora L.) it is possible to extract oil that has been utilized industrially, especially by cosmetics and pharmaceuticals sectors. The extraction of this oil by using conventional methods often causes the thermal degradation of its components, and an interesting alternative has been the use of supercritical extraction technology with organic solvents. In order to better evaluate the advantages of oil extracting from red and purple Surinam cherry s leaves in high pressure, the present paper aims to study this supercritical extraction by using the supercritical carbon dioxide and pressured n-propane as solvents. After drying and milling of red and purple Surinam cherry s leaves, they were underwent to oil extraction with CO2 supercritical fluids under different temperatures (50 and 60ºC) and the pressure (150 and 250 bar) and also n-propane in different temperature (30, 45 and 60ºC) and pressure conditions (40, 60 e 80 bar). The coupling of a fractionation column in supercritical fluid extraction was used to separate components of the extract. Three distinct stationeries phases were evaluated: silica, alumina and Amberlit®. The extracted oil underwent to a gas chromatography coupled to the mass spectrometry (CG-EM) for a quantitative analysis, showing the alpha-bisabolol as composed of greater interest in its industrial application. The extraction kinetics of both solvents were obtained in an experimentally way. The experimental data were adjusted appropriately to the mathematical Sovavá model.
Das folhas de pitanga (Eugenia uniflora L.) é possível extrair um óleo que tem sido bastante utilizado industrialmente, principalmente nos segmentos cosméticos e farmacêuticos. As extrações deste óleo utilizando os métodos convencionais geralmente causam a degradação térmica de seus componentes, e uma alternativa interessante tem sido a utilização da tecnologia de extração supercrítica com solventes orgânicos. Para avaliar melhor as vantagens da extração em pressões elevadas do óleo das folhas de pitanga de frutos vermelha e roxa, o presente trabalho teve como objetivo estudar este tipo de extração supercrítica utilizando como solventes o dióxido de carbono supercrítico e o n- propano pressurizado. Após secagem e moagem das folhas de pitanga vermelha e roxa, as mesmas foram submetidas à extração do óleo com os solventes CO2 supercrítico sob diferentes condições de temperatura (50 e 60°C) e de pressão (150 e 250 bar) e também n-propano em diferentes condições de temperatura (30, 45 e 60°C) e de pressão (40, 60 e 80 bar). O acoplamento de uma coluna de fracionamento na extração supercrítica foi usado para separar os componentes do extrato. Foram avaliadas 3 fases estacionárias distintas: sílica, alumina e Amberlit®. O óleo extraído foi submetido à cromatografia gasosa acoplado a espectrometria de massa (CG-EM) para análise qualitativa, apresentado o alfa-bisabolol como composto de maior interesse pela sua aplicação industrial. A cinética da extração de ambos os solventes foram obtidas de forma experimental. Os dados experimentais ajustaram-se adequadamente ao modelo matemático de Sovová.

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Pederssetti, Marcia Mantovani. "Análise dos efeitos da temperatura e pressão na extração supercrítica do óleo essencial de canola com dióxido de carbono supercrítico e n-propano pressurizado." Universidade Estadual do Oeste do Parana, 2008. http://tede.unioeste.br:8080/tede/handle/tede/1880.

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Currently it is possible to observe a great interest in the consumption of canola oil due to medical and nutritionist indication as a functional food for people who are interested in a healthy diet, for the reason of its excellent composition of fatty acid. The most common employed process to the canola oil extraction is the use of organic solvents, normally it is used the n-hexane that is toxic, flammable, coming from non-renewable source and hazardous to the employees health. Pharmaceutical products, food and cosmetics can be got with the use of a solvent in the supercritical phase with the advantage of using non-toxic solvents and of working on very relatively low temperatures, being easily separated of the final product due to its high volatility, resulting in higher increase and selectivity to the ones found in the conventional processes. This work had as objective to study the behavior of canola solubility by using supercritical CO2 and pressurized n-propane in different experimental conditions and comparing to the conventional extraction. The operational conditions by using the supercritical CO2 as a solvent were: the temperatures of 40, 50 e 60 ºC and pressure of 20, 22,5 e 25 MPa. For the npropane solvent were established temperatures of 30, 45 e 60 ºC and pressure of 8, 10 e 12 MPa. The experimental planning applied on this study was the Factorial Planning with a central point of the type 22. The extracted samples in the different operational conditions were submitted to the oxidative stability analysis through the techniques of Exploratory Differential Calorimeter. It was accomplished the protein analysis of a bran. It was also accomplished a mathematical model through of a second order empirical model and the model of Sovová, to the experimental data obtained in the extraction with CO2 e n-propane. The results for the extraction by using the CO2 as a solvent have shown that the canola oil is more soluble in low temperature and high-pressure conditions. For the pressurized n-propane solvent, the best mass increase has occurred in the condition of higher temperature and pressure. The time for extraction with the n-propane was considerable shorter when compared to other solvents, being a better solvent to be used in the extraction of the canola oil. The conventional extraction with n-hexane has presented a high increase, even though the extraction has happened within a time of 20 hours, much higher when compared to the time of extraction using the supercritical CO2 and the pressurized n-propane. In the oxidative stability analysis of the oils was observed that the obtained oils within the three methods of extraction presented a good time of oxidative induction. The analysis done with the pies have shown that the values between the solvents CO2 and n-propane form next, just changing from the extracted pies with n-hexane, however the time of extraction with this solvent was higher when compared to the others. The mathematical model of a second order as the Sovová model, applied to the experimental data in the extraction with supercritical CO2 and pressurized n-propane, in all the operational conditions has adjusted to the canola oil.
Nos dias atuais observa-se um grande interesse no consumo do óleo de canola devido à indicação por médicos e nutricionistas como alimento funcional para pessoas interessadas em uma dieta saudável em razão da sua excelente composição de ácidos graxos. O processo mais comumente utilizado para a extração do óleo de canola é a utilização de solventes orgânicos, geralmente é usado o n-hexano que é tóxico, inflamável, provindo de fonte não renovável e perigosa a saúde de funcionários. Produtos farmacêuticos, alimentícios e cosméticos podem ser obtidos através do uso de um solvente na fase supercrítica com as vantagens de se utilizar solventes atóxicos e de se trabalhar a temperaturas relativamente baixas, sendo facilmente separado do produto final, devido a sua alta volatilidade, resultando em rendimento e seletividades superiores aos obtidos nos processos convencionais. Este trabalho teve como objetivo estudar o comportamento da solubilidade da canola, utilizando CO2 supercrítico e n-propano pressurizado, em diferentes condições experimentais e comparar com a extração convencional. As condições operacionais utilizando o CO2 supercrítico como solvente foram: temperaturas de 40, 50 e 60 ºC e pressões de 20, 22,5 e 25 MPa. Para o solvente n-propano foram estabelecidas temperaturas de 30, 45 e 60 ºC e pressões de 8, 10 e 12 MPa. O planejamento experimental utilizado nesse estudo foi o Planejamento Fatorial com ponto central do tipo 22. As amostras de óleo extraídas nas diferentes condições operacionais foram submetidas à análise de estabilidade oxidativa através da técnica de Calorimetria Diferencial Exploratória. Realizou-se também análise de proteína da torta. Foi realizada a modelagem matemática através de um modelo empírico de segunda ordem e do modelo de Sovová, para os dados experimentais obtidos nas extrações com CO2 e n-propano. Os resultados para as extrações utilizando o CO2 como solvente mostraram que o óleo de canola é mais solúvel em condições de baixa temperatura e pressão elevada. Para o solvente npropano pressurizado, o melhor rendimento de massa ocorreu na condição de maior temperatura e pressão. O tempo de extração com n-propano foi consideravelmente menor quando comparado aos outros solventes, se mostrando um melhor solvente a ser utilizado na extração do óleo de canola. A extração convencional com n-hexano apresentou um alto rendimento, no entanto a extração ocorreu em um tempo de 20 horas, muito acima quando comparado ao tempo de extração utilizando o CO2 supercrítico e n-propano pressurizado. Na análise da estabilidade oxidativa dos óleos, observou-se que os óleos obtidos nos três métodos de extração apresentaram um bom tempo de indução oxidativa. As análises de proteína realizadas nas tortas demonstraram que os valores entre os solventes CO2 e npropano foram próximos, diferindo apenas das tortas extraídas com n-hexano, porém o tempo de extração com esse solvente foi maior quando comparado aos demais. O modelo matemático de segunda ordem, assim como o modelo de Sovová, aplicado aos dados experimentais na extração com CO2 supercrítico e n-propano pressurizado, se ajustaram em todas as condições operacionais para a extração do óleo de canola.

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Ribas, Marielen Cozer. "Estudo do processo combinado de extração em altas pressões e purificação do óleo de candeia pelo processo de adsorção em coluna de leito fixo." Universidade Estadual do Oeste do Parana, 2012. http://tede.unioeste.br:8080/tede/handle/tede/1830.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico
The Candeia (Eremanthus erythropappus) has a rich oil in α-bisabolol, a substance of high commercial value and wide industrial application. An alternative to traditional methods of extraction and / or fractionation of the candeia oil is the use of supercritical technology, with the advantage of not having the disadvantages of thermal degradation and the use of organic solvents. Thus, this research aims to evaluate the combined process of supercritical extraction and purification of the candeia oil by adsorption in fixed bed column. For the extractor packaging were used 42g of candeia wood with a particle size from 28 to 32 mesh. For the extraction were evaluated two solvents, supercritical carbon dioxide and propane pressurized. The experiments were conducted at temperatures of 40, 50 and 60 °C and pressures of 100, 120, 150, 200 and 245 bar for carbon dioxide. For propane, the temperature conditions studied were 30, 55 and 80 °C and pressures of 80, 100 and 120 bar; for the experiments with propane was performed a 22 factorial design with the focal point in triplicate. The effect of the temperature and pressure in the ratio of oil mass extracted per mass of solvent was evaluated for the different experimental conditions. For carbon dioxide the condition with the highest yield was at 60 ° C and 245 bar, while for propane, the best condition was 60 ° C and 80 bar. As the ratio of oil mass / solvent mass, the best operating conditions are 40 º C and 200 bar for CO 2 and 80 ° C and 80 bar for propane. From the experimental data of the kinetics of extraction, the mathematical model of Sovová was tested, which satisfactorily represented the experimental data. The results showed that extraction with pressurized propane presented higher extraction rate and content of α-bisabolol when compared to carbon dioxide, dichloromethane and hexane, indicating that propane is the most appropriate solvent for the extraction of oil from the candeia wood. To obtain a rich oil in -bisabolol a purification was performed under income yield higher conditions. Of the tested adsorbents, the silica gel presented greater capacity for purification of the extract than alumina.
A Candeia (Eremanthus erythropappus) possui um óleo rico em α-bisabolol, substância de alto valor comercial e de grande aplicação industrial. Uma alternativa aos métodos tradicionais de extração e/ou fracionamento do óleo de candeia é a utilização da tecnologia supercrítica, com a vantagem de não ter os inconvenientes da degradação térmica e da utilização de solventes orgânicos. Sendo assim, esta pesquisa visa avaliar o processo combinado de extração supercrítica e purificação do óleo de candeia por meio da adsorção em coluna de leito fixo. Para o empacotamento do extrator foram utilizados 42g da madeira de candeia com granulometria de 28 a 32 mesh. Para a extração foram avaliados dois solventes, o dióxido de carbono supercrítico e o propano pressurizado. Os experimentos foram conduzidos em temperaturas de 40, 50 e 60 oC e pressões de 100, 120, 150, 200 e 245 bar para o dióxido de carbono. Para o propano, as condições estudadas de temperatura foram 30, 55 e 80 oC e pressões de 80, 100 e 120 bar; para os experimentos com propano foi realizado um planejamento fatorial 22 com triplicata no ponto central. Avaliou-se o efeito da temperatura e pressão na razão de massa de óleo extraída por massa de solvente utilizado para as diferentes condições experimentais. Para o dióxido de carbono, a condição que apresentou maior rendimento foi a de 60 oC e 245 bar, enquanto que para o propano, a melhor condição foi de 60 oC e 80 bar. Quanto a razão massa de óleo/massa de solvente, melhores condições de operação são de 40 ºC e 200 bar para o CO2 e 80 ºC e 80 bar para o propano. A partir dos dados experimentais das cinéticas de extrações foi testado o modelo matemático de Sovová, que representou satisfatoriamente os dados experimentais. Os resultados mostraram que extrações com propano pressurizado apresentaram maior taxa de extração e teor de α-bisabolol quando comparado ao dióxido de carbono, diclorometano e ao hexano, indicando que o propano é um solvente mais apropriado para extração do óleo da madeira de candeia. Para se obter um óleo rico em -bisabolol uma purificação foi realizada, nas condições de maior rendimento. Dos adsorventes testados, a sílica gel apresentou maior capacidade de purificação do extrato do que a alumina.

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GideonEffendi, Petrick, and 黃敏獅. "Study on Recovery of Nonionic Surfactants by Solvent Extraction after Surfactant-Based Extraction Processes." Thesis, 2011. http://ndltd.ncl.edu.tw/handle/60300843438629892098.

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Ferreira, Ana Maria da Conceição. "Ionic liquids aqueous solutions as sustainable solvents in separation processes." Doctoral thesis, 2018. http://hdl.handle.net/10773/24094.

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This work is focused on the development of sustainable and cost-effective solvents and separation processes, particularly by applying aqueous solutions of ionic liquids (ILs). It is shown the potential of ILs aqueous solutions as alternative solvents to extract value-added compounds from biomass, avoiding the use of the commonly applied volatile organic solvents, and their use as phase-forming components of aqueous biphasic systems (ABS) to develop reversible and/or integrated separation platforms. In the first set of results, it is demonstrated the high performance of ILs aqueous solutions to extract caffeine and hydroxymatairesinol (HMR) from spent coffee grounds (SCG) and Norway spruce knots, respectively. In the first work it is shown the relevance of the hydrotropy concept as the major factor behind the improved extraction performance of ILs aqueous solutions, whereas in the second work biocompatible ILs were applied and proposed to be used directly with the biomass extracts in nutraceutical and cosmetic applications. Still focused on the use of ILs aqueous solutions, these were then explored in the creation of reversible aqueous biphasic systems (ABS) as alternative separation platforms, followed by the development of integrated production-separation strategies. Transitions from monophasic to biphasic regimes were shown to occur by changes in pH and temperature (applied as external stimulus). Examples on their use in the separation of mixtures of amino acids and of nucleic acids from proteins are given. Finally, it is shown the applicability of reversible ABS as integrated production-separation processes. pH-driven ABS were applied in the production of hydroxymethylfurfural (HMF) from fructose at acidic media, followed by their separation at alkaline conditions (inducing the two phases separation). On the other hand, and taking advantage of the biocompatible nature of the ABS phase-forming components, thermoreversible ABS were used in biocatalytic processes. A reaction catalysed by laccase occurs in the homogenous solution, after which small temperature changes induce the two-phase formation and the complete separation of the enzyme from the respective product. These systems also allow the recovery and reuse of the ABS phases, contributing towards the development of sustainable production and separation processes. Although additional research on these solvents and systems scale-up feasibility is still required, the results here presented unveil the relevance of IL aqueous solutions as alternative solvents and on the development of efficient separation processes
Este trabalho compreende o desenvolvimento de solventes e processos de separação sustentáveis, eficientes e rentáveis, através da aplicação de soluções aquosas de líquidos iónicos (LIs). Em particular mostra-se o potencial de soluções aquosas de LIs como solventes alternativos para a extração de compostos de valor acrescentado a partir de biomassa, evitando portanto a utilização de solventes orgânicos voláteis, assim como a sua utilização na formação de sistemas aquosos bifásicos (SAB) como processos de separação. No primeiro conjunto de resultados demonstra-se que soluções aquosas de LIs apresentam uma elevada capacidade para extrair cafeína e hidroximatairesinol (HMR) de borras de café e de nós de abeto da Noruega, respetivamente. O primeiro trabalho nesta vertente mostra a importância do conceito de hidrotropia, atuando como o principal fator responsável pelo elevado desempenho das soluções aquosas de LIs na extração de compostos de valor acrescentado a partir de biomassa, enquanto que o segundo trabalho demonstra a utilização de LIs biocompatíveis, permitindo a utilização direta dos extratos de biomassa em aplicações nutracêuticas e de cosmética. As soluções aquosas de LIs também foram estudadas na criação de SAB reversíveis, como plataformas de separação alternativas, assim como no desenvolvimento de sistemas integrados de reação-separação. As respetivas transições de fase ocorrem por aplicação de estímulos externos, tais como pH e temperatura, e a sua aplicação foi demonstrada na separação de misturas de aminoácidos, e ácidos nucleicos e proteínas. Por fim, demonstra-se a utilização de SAB reversíveis como processos integrados de produção e separação. Os SAB reversíveis obtidos por alterações de pH foram aplicados na produção de hidroximetilfurfural (HMF) a partir de frutose em meio ácido, seguido da sua separação em condições alcalinas (induzindo a formação de duas fases). Por outro lado, e tirando partido da natureza biocompatível dos constituintes dos SAB, estudaram-se SAB reversíveis através da alteração da temperatura em processos biocatalíticos. A reação ocorre em meio homogéneo, catalisada pela lacase, onde pequenas alterações de temperatura induzem a formação de duas fases e a completa separação da enzima do respetivo produto. Estes sistemas permitem também a recuperação e reutilização das fases/constituintes dos SAB, contribuindo para o desenvolvimento de processos sustentáveis. Embora seja ainda necessária investigação adicional sobre a viabilidade destes solventes e sistemas para aplicação em larga escala, os resultados aqui apresentados mostram a relevância de soluções aquosas de LIs como solventes alternativos e no desenvolvimento de processos de separação
Programa Doutoral em Engenharia Química

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Cheng, Hou-Chieh, and 程厚捷. "Computer-Aided Solvent Design for Extractive Fermentation Processes with Cell-recycling." Thesis, 2007. http://ndltd.ncl.edu.tw/handle/12297184056097072527.

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博士
國立中正大學
化學工程所
96
In this study, a systematic framework for the design and analysis of solvents in extractive fermentation-distillation systems is developed using a computer-aided molecular design (CAMD) technique. The article framework consists of performances of fermentation process, solvent evaluation, and solution strategy approaches. Bioethanol is a bulk chemical and must carry out continuous fermentation to achieve economic and beneficial production. Achieving high productivity of ethanol continuous fermentation requires retaining high cell density culture and maximizing the dilution rate. Continuous fermentation with cell recycling can increase ethanol productivity; however, such a high ethanol concentration may poison viable microorganisms and abrogate the fermentation process. Extractive fermentation is a technique that solvent can be used to reduce the end product inhibition through the use of water-immiscible phase that removes the fermentation product in situ. However, the toxicity of the organic solvent used to remove the end product in reaction media is always a problem. A good selection of the solvent will definitely benefit the fermentation process. In this study, crisp and fuzzy optimization approaches are respectively introduced to design an optimal biocompatible solvent for an extractive fermentation process. The optimal design problem is formulated as a mixed-integer nonlinear programming model in which performance requirements of the compounds are reflected in the objective and the constraints. In general, the requirements for the objective and constraints are not rigid; consequently, the fuzzy optimization approach is applied to soften the rigid requirement for maximization of the extraction efficiency and to consider the mass flow rate of solvent as the softened inequality constraints to the solvent design problem. Having elicited the membership function for the objective function and the constraint, the optimal solvent design problem can be formulated as a fuzzy goal attainment problem. Mixed-integer hybrid differential evolution is applied to solve the problem in order to find a satisfactory design. When designing a biocompatible solvent for the extractive fermentation process, many issues, such as extractive efficiency, conversion, amount of solvent utilized and so on, have to be considered. An interactive multiple-goal design procedure is introduced to determine a trade-off result in order to satisfy such contradicted goals. In this study, crisp and fuzzy multiple-goal optimization approaches are respectively introduced to design an optimal biocompatible solvent to a two-stage extractive fermentation with cell recycling for ethanol production. Both approaches could be iterated to solve the interactive multiple goal design problem in order to yield a trade-off result. However, the crisp optimization design is a tedious task that requires the designer to provide various pairs of the upper bounds for the design problem to obtain the corresponding solution. The fuzzy optimization approach is able to be trade-off several goals simultaneously and to yield the overall satisfactory grade for the product/process design problem. For achieving high ethanol productivity, we compare the process performance between single and double stage extractive fermentation with cell-recycling. The double stage process could use a smaller amount of fresh solvent to increase more ethanol productivity than that of the single stage process, but this would also decrease overall conversion. Comparing the two designs for the double stage process, process design and the simultaneous process/solvent design, the simultaneous design could yield higher overall ethanol productivity than the process design. Moreover, the maximum ethanol production rate of the double-stage extractive fermentation with cell recycling was about ten-fold higher than that of the continuous fermentation and about two-fold higher than the continuous fermentation with cell recycling. Based on anhydrous ethanol production of great bulk, besides raising the ethanol production rate by extractive fermentation technique, it is still a great challenge how to purify fermentation product that mainly consist of ethanol/water mixture forms a minimum-boiling azeotrope. For the standpoint of solvent characteristics, the use of an extractive solvent similarly could also enhance the volatility difference between the components to be separated in distillation column. In the other word, extractive distillation is an alternative technique for purifying ethanol fermented product in order to achieve anhydrous ethanol production. In this study, using CAMD technique is proposed to design suitable solvents for an integrated extractive fermentation and extractive distillation process in order to achieve anhydrous ethanol production.

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Chiou, Ming-Hao. "Process Simulation and Evaluation of Alternative Solvents for Jatropha Curcas L. Seed Oil Extraction in Biodiesel Production." Thesis, 2011. http://hdl.handle.net/1969.1/ETD-TAMU-2011-08-9205.

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Jatropha curcas L. is a drought-resistant plant which can be grown in poor soil and marginal lands. The use of Jatropha seed oil to produce biodiesel has been widely studied in recent years. Results showed that it is one of the most promising alternatives for conventional petro-diesel. Currently, hexane is still the most commonly used solvent for commercial oil extraction. However, the increasing price and flammability properties of hexane are motivating industry to seek alternative solvents. The objectives of this study are to design and analyze the Jatropha seed oil extraction for use in biodiesel production, and to provide a systematic safety-economic analysis of alternative solvents that can be used in Jatropha seed oil extraction. First, a base-case flowsheet is synthesized for oil extraction. Then, the base-case extraction process and each solvent Fire and Explosion Index (F & EI) and the Solvent Safety Index (SSI). Eight solvents, including n-heptane, toluene, xylene, dichloromethane, chloroform, 1,2-dichloroethane, methanol and ethanol are selected for candidates by comparing these results to those for hexane. Two cases are developed to evaluate the economic potential of these candidates. Furthermore, heat integration is applied to the process to minimize energy usage. Finally, a comprehensive solvent comparison is developed based on F & EI, SSI, solvent makeup cost, utilities cost, and capital investment. The results show that chloroform is the optimal solvent, while dichloromethane is the next best.

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Bastos, João António Pereira de Carvalho. "Modelagem de processos de destilação extractiva : selecção de solventes, simulação e integração energética." Tese, 1987. http://hdl.handle.net/10216/12240.

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Bastos, João António Pereira de Carvalho. "Modelagem de processos de destilação extractiva : selecção de solventes, simulação e integração energética." Doctoral thesis, 1987. http://hdl.handle.net/10216/12240.

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Sousa, Ana Maria do Sacramento Lopes. "Valorização de resíduos da indústria vinícola através de processos de extração por solventes." Master's thesis, 2020. http://hdl.handle.net/10316/92283.

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Dissertação de Mestrado Integrado em Engenharia Química apresentada à Faculdade de Ciências e Tecnologia
A indústria vinícola é um setor de atividade muito importante em Portugal e no mundo, gerando elevadas quantidades de resíduos sólidos e líquidos. O bagaço de uva é um dos resíduos sólidos resultantes do processo de vinificação que é rico em compostos de valor acrescentado, os polifenóis. Estes compostos são uma classe de metabolitos produzidos pelas plantas, com elevado poder antioxidante, e com inúmeros benefícios biológicos, podendo ser utilizados na indústria alimentar ou farmacêutica. O objetivo deste trabalho consistiu na análise da possibilidade de valorização do bagaço de uva por processos de extração com solvente, de modo a recuperar os polifenóis. O resíduo foi caracterizado física e quimicamente e realizaram-se ensaios preliminares com cinco solventes, a diferentes tempos de operação, temperatura e pH para estudar o comportamento do sistema de extração. A extração de compostos fenólicos foi otimizada mediante um desenho de experiências (DoE), para a acetona e o etanol, variando a temperatura, o tempo de contacto, a concentração de solvente e a razão sólido-líquido (L/S). O resíduo estudado tem características muito semelhantes às reportadas na literatura. As condições ótimas de extração foram identificadas, correspondendo a um tempo de 1,5 h, concentração do solvente em 50 % (v/v) e razão L/S igual a 25 mL/g. Para o etanol, a temperatura de operação ótima foi de 60 ºC, o que permitiu uma recuperação de polifenóis de 40,4 mg GAE/ g TS. Para a acetona, a temperatura ótima correspondeu a 50 ºC, recuperando-se 54,6 mg GAE/ g TS. Este trabalho permitiu concluir que a extração é favorecida usando misturas de um solvente orgânico e água, geralmente, em proporções próximas de 50 % (v/v), pelo aumento da temperatura até um limite máximo de 60 / 70 ºC, pelo aumento do tempo de extração e por razões L/S entre 20 e 30 mL/g. Concluiu-se que dos solventes estudados, a acetona é o que permite recuperar maior quantidade de polifenóis, mesmo usando temperaturas mais baixas que nas extrações que o etanol.
The wine industry is a very important industrial sector in Portugal and in the world, producing high amounts of solid and liquid wastes. Grape pomace is one of the solid wastes produced during the wine making process and it is rich in polyphenols, which are valuable compounds. Polyphenols are a family of molecules commonly produced by plants, with high antioxidant capacity and several biological functions, which can be used in the food and pharmaceutical industries. The main objective of this work was the analysis of the valorization of grape marc through processes of extraction with solvents for recovering polyphenols. The residue was characterized in terms of the main physical and chemical parameters and preliminary assays were conducted with five different solvents, to understand the behavior of the extraction system as a function of time, temperature, and pH. The extraction of polyphenols was optimized using a design of experiments approach (DoE), based on the Central Composite Design. Ethanol and acetone were the solvents investigated. The operating variables considered were temperature, contact time, solvent concentration, and solid-liquid ratio (L/S). The characterization showed that the physico-chemical parameters of the residue are very similar to those reported in the literature. The optimal conditions to operate the extraction were identified as: contact time of 1,5 h, solvent concentration 50 % (v/v), and L/S ratio 25 mL/g for both solvents. For ethanol, the optimal temperature was 60 ºC, which led to a polyphenol recovery of 40,4 mg GAE/ g TS. For acetone, the optimal temperature was 50 ºC, with a polyphenol recovery of 54,6 mg GAE/ g TS. With this work, it was concluded that the extraction is improved with the use of a mixture of water and an organic solvent, with the proportion of the organic solvent rounding 50 %, with the increase of temperature up to a limit between 60 and 70 ºC, with the increase of the extraction time and with L/S ratios between 20 and 30 mL/g. Moreover, acetone was the best solvent with higher polyphenol recuperations, even using lower temperatures than those practiced with ethanol.

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Detcheberry, Mylene. "Valorisation chimique des condensats issus de la torréfaction de biomasses : modélisation thermodynamique, conception et analyse des procédés." Thesis, 2015. http://www.theses.fr/2015INPT0131/document.

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Abstract:

La biomasse lignocellulosique est considérée comme une ressource de carbone renouvelable possédant un grand potentiel pour la une valorisation énergétique et chimique. La torréfaction de la biomasse sèche (de type bois) est un procédé de transformation thermique s’effectuant à des températures comprises entre 200°C et 300°C, et un temps de séjour compris entre quelques minutes et plusieurs heures, opérant sous pression atmosphérique et en défaut d’air. Le produit principal de la torréfaction est un combustible solide hydrophobe et stable. Cette opération génère des coproduits gazeux à haute température qui sont habituellement considérés comme des effluents pénalisants, apportant au mieux un appoint d’énergie pour le procédé. Pourtant, de nombreux constituants présents dans les condensats – récupérés par condensation des coproduits de torréfaction – pourraient être valorisés comme produits chimiques bio-sourcés. L'objectif de la thèse est de proposer un procédé de séparation-purification pour les composés condensables présents dans ces effluents gazeux. Ces condensats constituent une phase majoritairement aqueuse, contenant plus de 150 espèces organiques identifiées. Les espèces minoritaires sont présentes dans des proportions variables suivant le bois torréfié. Enfin il s’agit d’un mélange réactif et thermiquement instable, où différents équilibres chimiques sont présents. Une analyse des caractéristiques physico-chimiques des condensats a permis de proposer un milieu modèle limité à une dizaine de composés. Un modèle représentatif du comportement thermodynamique de ce mélange réactif à large spectre de masse moléculaire a été sélectionné et les paramètres d’interaction binaire identifiés. Des données expérimentales d’équilibres liquide-vapeur ont été acquises pour valider en partie ce modèle. Les composés cibles et les objectifs du procédé de valorisation ont été choisis et plusieurs stratégies de valorisation ont été élaborées et simulées sous Prosim+ sur la base de la modélisation thermodynamique. Cette étude a permis d’évaluer ces différentes stratégies en termes d’efficacité énergétique et de pureté des produits finaux pour une potentielle mise en place à l’échelle industrielle de cette filière
Lignocellulosic biomass is considered as a renewable carbon resource with great potential for the energy and chemical recovery. Torrefaction is a thermal process carried out at temperatures below 300°C, under inert atmosphere, at atmospheric pressure, and with residence times for the solid biomass ranging from few minutes to several hours. Torrefied wood is a solid product constituted by more than 70% of the initial mass with properties close to those of coal. The 30% remaining part is a gaseous effluent, composed of about one third of non-condensable gases – carbon monoxide and carbon dioxide – and two thirds of condensable species. Currently, torrefied wood is the main product of interest and is usually transformed into energetic gases by the gasification process or directly used as coal for combustion. Conversely, gaseous by-products are considered at present time as a waste and in the best case are burned to provide energy to the process. Yet, the recovery and valorization of the condensable fraction as bio-sourced chemicals is worth considering. The aim of the thesis is to propose a separation-purification process for condensable chemicals of the waste gas. This condensable fraction is a predominantly aqueous phase, containing more than 150 identified organic species. Minority species are present in varying proportions depending on torrefied wood. Finally, it is a reactive and thermally unstable mixture, where different chemical equilibria are present. An analysis of the physicochemical characteristics of the condensable fraction allowed selecting a limited number of compounds to model the mixture. A representative model of the thermodynamic behavior of the reactive mixture has been selected and the binary interaction parameters identified. Experimental vapor-liquid equilibria data were acquired in part to validate this model. The target compounds and objectives of the recovery process were selected and several development strategies were developed and simulated in ProSim+ on the basis of thermodynamic modeling. This study assessed these different strategies in terms of energy efficiency and purity of the products for potential implementation on an industrial scale of this sector

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Dissertations / Theses on the topic 'Solvent extraction processes'

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