Dissertations / Theses on the topic 'Crystallization – Sugar'

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
Brazil is the largest producer of cane sugar and the largest producer and exporter of sugar being the state of São Paulo the responsible for over 60% of the national production of sugar, and the region is where is located the city of São Carlos is main producer region of Brazil, this fact becomes a motivation for this project. The crystallization process is the most important in the production of sugar and responsible for the quality of the final product. This work deals with the modeling and simulation of this process through three different approaches: the ideal crystallizer (MSMPR), the integrated sugar production without description of crystals, approach called "gray-box", and the industrial crystallizer. The models were developed in the software EMSO. The EMSO is a program developed in Brazil and has a great advantage compared to other programs, it's a free program, without the need to license purchase. By allowing full access to the developed mathematical models, facilitates the insertion of new models such as the present study about crystallization and allow the improvement of existing models, allowing also the development of specific software libraries. The first held approach, MSMPR, aims to introduce a protocol currents description containing solids and the crystallization process in the EMSO, for in his library there is no model that describes the crystallization or even containing solids, unlike other widely used commercial programs for the simulation of processes such as Aspen Plus, having a model MSMPR. So when performing this first approach, the EMSO can match other programs in relation to the crystallization process. The mass averaged crystal size (MA) obtained with the parameters set as default, L43 = 1.18 mm is much greater than the expected value L43 = 0.5 to 0.55 mm, but with the variation of the kinetic parameters can be obtained results within the desired range . The second approach is a simplified model called "gray-box" in order to facilitate the paying in of crystallization models with models referring to others process. The sugar production obtained in this model was similar than that reported in the literature, but the model can be useful in paying in of process models which constitute a industrial plant. The third and most important approach corresponds to the model of an industrial crystalliser with intent to represent real process of sugar production using data from literature. The discussion was carried out on the variables: temperature, brix, crystal mass and MA. The variations of temperature and brix relative to time obtained are consistent with each step of the process. The crystal mass produced in the simulation is approximately 50% lower than that found in the literature, whereas the MA is also below, but achieves excellent results in the change of the kinetic parameters. The final results obtained in the simulations do not coincide with the expected results, but the easy access to developed models makes these models a good instrument to parameters analysis, reaching with some changes in the kinetic parameters, in satisfactory results that well represent the real process.
O Brasil é o maior produtor mundial de cana-de-açúcar e o maior produtor e exportador de açúcar sendo que o estado de São Paulo é responsável por mais de 60% da produção nacional de açúcar, sendo o interior paulista a principal região produtora do Brasil, tal fato torna-se uma motivação para o presente projeto, pois é onde localiza-se a cidade de São Carlos. A etapa de cristalização é a mais importante na produção de açúcar, por ser a responsável pela qualidade do produto final. O presente trabalho trata da modelagem e simulação desse processo através de três diferentes abordagens: o cristalizador ideal (MSMPR), o processo integrado de produção de açúcar sem descrição dos cristais, abordagem denominada “caixacinza”, e o cristalizador industrial. Os modelos foram desenvolvidos no software EMSO. O EMSO é um programa desenvolvido no Brasil e possui um grande diferencial em relação aos demais programas de ser de uso gratuito, sem a necessidade de compra de licença. Por possibilitar acesso total aos modelos matemáticos desenvolvidos, facilita a inserção de novos modelos, como os de cristalização do presente trabalho e permitem o aprimoramento de modelos já existentes, possibilitando, ainda, o desenvolvimento de bibliotecas específicas no software. A primeira abordagem realizada, o MSMPR, tem como objetivo introduzir um protocolo de descrição de correntes contendo sólidos e o processo de cristalização no EMSO, pois em sua biblioteca não existe nenhum modelo que descreva a cristalização ou até mesmo que contenha sólidos, diferente de outros programas comerciais muito utilizados para a simulação de processos, como o Aspen Plus, que possui um modelo de MSMPR. Então ao realizar essa primeira abordagem o EMSO pode se igualar a outros programas em relação ao processo de cristalização. O tamanho médio mássico obtido com os parâmetros estabelecidos como padrão, L43 = 1,18 mm é muito maior que o valor esperado L43 = 0,5 a 0,55 mm, porém com a variação dos parâmetros cinéticos os resultados obtidos estão na faixa desejada. A segunda abordagem trata de um modelo simplificado denominado “caixa-cinza” com o objetivo de facilitar a integralização da cristalização com modelos referentes a outros processos. A produção de açúcar obtida nesse modelo foi similar à apresentada na literatura, sendo assim, o modelo pode ser útil em uma estimativa de produção do processo e na integralização de modelos de processos que constituem uma usina. A terceira e mais importante abordagem corresponde ao modelo de um cristalizador industrial, com a intenção de representar o processo real na produção de açúcar utilizando dados provenientes da literatura. A discussão dos resultados procedeu-se sobre as variáveis: temperatura, brix, massa de cristais e tamanho médio mássico. As variações da temperatura e do brix em relação ao tempo obtidas condizem com cada etapa do processo. A massa de cristal produzida na simulação é proximadamente 50% menor do que a encontrada na literatura, enquanto que o tamanho médio também está abaixo mas atinge ótimos resultados com a alteração dos parâmetros cinéticos. Os resultados finais obtidos nas simulações não coincidiram com os resultados esperados, porém o fácil acesso aos modelos desenvolvidos torna esses modelos bons instrumentos de análises de parâmetros, podendo chegar com algumas mudanças nos parâmetros cinéticos, a resultados satisfatórios que representem bem o processo real.

Utilizing Phase Change Materials (PCM) for Latent Thermal Energy Storage (LTES) applications have previously been extensively researched as a measure to reduce greenhouse gas emissions from energy consumption. In order to make use of the waste heat from industrial processes for LTES purposes, a new demand emerged for PCMs capable of phase change in mid-temperature ranges of 100 °C - 200 °C. This higher temperature requirement made most of the previously studied material inapplicable as they had much lower melting and solidification temperatures. With this in mind, a new generation of PCMs consisting of Sugar Alcohols (SA) has been proposed. Erythritol is seen as an especially promising SA with good thermophysical properties for LTES purposes. However, it has been shown to suffer from severe supercooling, which makes it unreliable in real applications. To eradicate this issue, two additives, Graphene Oxide (GO) and Polyvinylpyrrolidone (PVP) at varying mass fractions were mixed with pure erythritol to form a composite which was studied using the Temperature-history (T-history) method to determine its effectiveness in reducing supercooling. Results show that at its most effective mass fraction, GO reduces supercooling by 28 o C and a 31 o C reduction is seen by the addition of PVP. The impacts on the duration of crystallization was also documented and analyzed using the same method. It was observed that the duration of crystallization was increased with increasing mass fractions of the additives. Other important properties of the composites were also studied in order to determine the overall feasibility for industrial applications. It includes analysis of the storage capacity through latent heat, changes in viscosity along with impacts on thermal diffusivity of the composites.
Att använda fasändringsmaterial (PCM) för termisk energilagring i form av latent värme (LTES) har tidigare extensivt forskats och undersökts som en lösning för att minska utsläppen av växthusgaser från energiförbrukning. För att utnyttja spillvärme från industriella processer för LTES-ändamål uppstod en efterfrågan på PCM som ändrar fas i temperaturer mellan 100 °C - 200 °C. Detta krav på högre temperatur gjorde att de flesta av de tidigare aktuella materialen inte kunde tillämpas eftersom de hade mycket lägre smält- och kristalliseringstemperaturer. Med detta i åtanke har en ny generation av PCM bestående av sockeralkoholer (SA) föreslagits. Erytritol ses som ett särskilt lovande SA med goda egenskaper för LTES-ändamål. Den har dock visat sig drabbas av svår underkylning, vilket gör den opålitligt i verkliga tillämpningar. För att utrota detta problem blandades två tillsatser, Graphene Oxide (GO) och Polyvinylpyrrolidone (PVP) vid olika massfraktioner med ren erytritol för att bilda en komposit som studerades med metoden Temperature-history (T-history) för att bestämma dess effektivitet på att minska underkylningen. Resultaten visar att GO på sin mest effektiva massfraktion minskar underkylningen med 28 o C och tillsats av PVP lyckats minska den med som mest 31 o C. Påverkningarna på varaktighet av kristallisering dokumenterades och analyserades med samma metod. Det var observerad att varaktigheten av kristallisering ökades med ökande massfraktioner av tillsatserna. Även andra viktiga egenskaper hos kompositerna studerades för att avgöra rimligheten att använda dessa för industriella tillämpningar. Det inkluderar analys av lagringskapaciteten genom latent värme, förändringar i viskositet tillsammans med påverkan på kompositernas termiska diffusivitet.

Utilizing Phase Change Materials (PCM) for Latent Thermal Energy Storage (LTES) applications have previously been extensively researched as a measure to reduce greenhouse gas emissions from energy consumption. In order to make use of the waste heat from industrial processes for LTES purposes, a new demand emerged for PCMs capable of phase change in mid-temperature ranges of 100 °C - 200 °C. This higher temperature requirement made most of the previously studied material inapplicable as they had much lower melting and solidification temperatures. With this in mind, a new generation of PCMs consisting of Sugar Alcohols (SA) has been proposed. Erythritol is seen as an especially promising SA with good thermophysical properties for LTES purposes. However, it has been shown to suffer from severe supercooling, which makes it unreliable in real applications. To eradicate this issue, two additives, Graphene Oxide (GO) and Polyvinylpyrrolidone (PVP) at varying mass fractions were mixed with pure erythritol to form a composite which was studied using the Temperature-history (T-history) method to determine its effectiveness in reducing supercooling. Results show that at its most effective mass fraction, GO reduces supercooling by 28 oC and a 31 oC reduction is seen by the addition of PVP. The impacts on the duration of crystallization was also documented and analyzed using the same method. It was observed that the duration of crystallization was increased with increasing mass fractions of the additives. Other important properties of the composites were also studied in order to determine the overall feasibility for industrial applications. It includes analysis of the storage capacity through latent heat, changes in viscosity along with impacts on thermal diffusivity of the composites.
Att använda fasändringsmaterial (PCM) för termisk energilagring i form av latent värme (LTES) har tidigare extensivt forskats och undersökts som en lösning för att minska utsläppen av växthusgaser från energiförbrukning. För att utnyttja spillvärme från industriella processer för LTES-ändamål uppstod en efterfrågan på PCM som ändrar fas i temperaturer mellan 100 °C - 200 °C. Detta krav på högre temperatur gjorde att de flesta av de tidigare aktuella materialen inte kunde tillämpas eftersom de hade mycket lägre smält- och kristalliseringstemperaturer. Med detta i åtanke har en ny generation av PCM bestående av sockeralkoholer (SA) föreslagits. Erytritol ses som ett särskilt lovande SA med goda egenskaper för LTES-ändamål. Den har dock visat sig drabbas av svår underkylning, vilket gör den opålitligt i verkliga tillämpningar. För att utrota detta problem blandades två tillsatser, Graphene Oxide (GO) och Polyvinylpyrrolidone (PVP) vid olika massfraktioner med ren erytritol för att bilda en komposit som studerades med metoden Temperature-history (T-history) för att bestämma dess effektivitet på att minska underkylningen. Resultaten visar att GO på sin mest effektiva massfraktion minskar underkylningen med 28 oC och tillsats av PVP lyckats minska den med som mest 31 oC. Påverkningarna på varaktighet av kristallisering dokumenterades och analyserades med samma metod. Det var observerad att varaktigheten av kristallisering ökades med ökande massfraktioner av tillsatserna. Även andra viktiga egenskaper hos kompositerna studerades för att avgöra rimligheten att använda dessa för industriella tillämpningar. Det inkluderar analys av lagringskapaciteten genom latent värme, förändringar i viskositet tillsammans med påverkan på kompositernas termiska diffusivitet.

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Introduced during the colonial period in Brazil, nowadays sugar cane is one of the main crops of the country's economy, generating more than 2 billion dollars per year in the Brazilian trade balance. Despite the benefits of expanding the sugarcane sector every year, the environmental impacts caused by burning straw cane sugar made the State of São Paulo Government create the Protocol of Agro-Environmental Cooperation in 2007, which aims the total elimination of cane burning by 2017. However, when the sugar cane stops being burned, some components of the plant, which remained in the field due to the burning, will start being in larger quantities in the process, and the effects of this future reality in sugar quality have not been studied In this doctoral thesis, the two components of great impact on the specifications or quality of the sugar were chosen: starch and dextran which were studied in the crystallization unit operation (by controlled cooling and vacuum evaporation), so that the impact on the final product (sugar) were evaluated. This current study used a reponse surface methodology, with 2 levels (309 and 1062 ppm), two factors (dextran and starch), 3 center points (one central point in triplicate) and 4 axial points, totaling 11 trials per type of crystallization. The experiments were conducted with sugar Type 2 solutions contaminated with starch and dextran, in an agitated and jacketed crystallizer (8 liters) in the laboratory. When the crystallization was performed, the matters were centrifuged, the sugars were separated from the honeys, and forwarded to the physico-chemical, textural and optical microscopy analyzes. In relation to the physicochemical analyzes of sugar, starch and dextran contamination interfered directly in the responses: starch, dextran, color, turbidity and alcoholic floc in both crystallization techniques, however, the controlled cooling under the same conditions of contamination (0-2000 ppm), presented sugars to lower rates, which kept the product according to the market specifications. The results of grain size analysis showed frequency curves with accumulation of smaller crystals at the opening of 0.5 mm, according to the increase of dextran in the tests. And the optical microscopy analysis identified the existence of a relationship between the amount of contaminants, and the appearance of agglomerated crystals, besides "needle-like" crystals were not observed. The experimental chosen design collaborated in the identification of starch and dextran agents, in the increase or decrease of the analyzed responses, besides suggesting the collaboration of the combined effect on the quality of sugar. Concerning the product quality, the use of crystallization technique by controlled cooling proved to be the most suitable in the reduction of contaminants in the sugar, particularly in solutions containing 2,000 ppm of dextran and starch. Given the crop of sugarcane in the coming years, and that the contamination of dextran and starch may be higher than those found in syrups of industrial processes currently, this work may contribute to the knowledge of the contaminants and their combined actions in the crystallization and in understanding of the differences in the product quality.
Introduzida no período colonial no Brasil, a cana-de-açúcar é hoje uma das principais culturas da economia do país, gerando mais de 2 bilhões de dólares por ano na balança comercial brasileira. Apesar dos benefícios da expansão do setor sucroalcooleiro a cada ano, os impactos ambientais causados pelas queimadas da palha de cana-de-açúcar, levaram o Governo Estadual Paulista a criar em 2007, o Protocolo de Cooperação Agroambiental, que visa a eliminação total da queima de cana até 2017. No entanto, quando a cana-de-açúcar deixar de ser queimada, alguns componentes da planta que ficavam no campo com a queima passarão a entrar no processo em maiores quantidades, e os efeitos dessa futura realidade na qualidade do açúcar ainda não foram estudados. Nesse trabalho de doutorado, foram escolhidos dois componentes de grande impacto nas especificações ou qualidade do açúcar: o amido e a dextrana, os quais foram estudados na operação unitária de cristalização (por resfriamento controlado e por evaporação a vácuo), para que o impacto no produto final (açúcar) fosse avaliado. O presente trabalho utilizou um delineamento composto rotacional, com 2 níveis (309 e 1062 ppm), dois fatores (dextrana e amido), 3 pontos centrais (1 ponto central em triplicata) e 4 axiais, totalizando 11 experimentos por tipo de cristalização. Os experimentos foram realizados com soluções de açúcar Tipo 2, contaminadas com amido e dextrana, em um cristalizador agitado e encamisado (8 litros), em laboratório. Realizadas as cristalizações, as massas foram centrifugadas, e os açúcares separados dos méis, e encaminhados para as análises físico-químicas, granulométricas e de microscopia óptica. Em relação às análises físico-químicas do açúcar, as contaminações de dextrana e amido interferiram diretamente nas respostas: amido, dextrana, cor, floco alcoólico e turbidez, nas duas técnicas de cristalização, no entanto, o resfriamento controlado, nas mesmas condições de contaminação (0 a 2000 ppm), apresentou açúcares com os menores índices, o que manteve o produto nas especificações do mercado. Os resultados das análises granulométricas demonstraram curvas de frequência com acúmulo de cristais menores na abertura de 0,5 mm, conforme o aumento de dextrana nos testes. E as análises de microscopia óptica identificaram a existência de uma relação entre a quantidade de contaminantes, e o aparecimento dos cristais aglomerados, além de não serem observados cristais tipo agulha . O planejamento experimental adotado colaborou na identificação dos agentes amido e dextrana, no aumento ou na diminuição das respostas analisadas, além de sugerir a colaboração do efeito combinado desses na qualidade do açúcar. Em termos de qualidade do produto, a aplicação da técnica de cristalização por resfriamento controlado mostrou-se mais indicada na redução dos contaminantes no açúcar, principalmente em soluções com 2000 ppm de dextrana e amido. Tendo em vista a colheita de cana crua nos próximos anos, e que as contaminações de dextrana e amido poderão ser superiores as encontradas nos xaropes dos processos industriais hoje, o presente trabalho pode contribuir no conhecimento dos contaminantes e de suas ações combinadas na cristalização, e no entendimento das diferenças na qualidade do produto.

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Today, Brazil is the major producer and exporter of sugar in the world. In the last harvest 2008/2009, 31.5 millions tons were produced, of which 60% were exported providing a 40% of international market share. However, sugar is a product that has commercial difficulties, due to the hard restrictions, such as rates, subsidizes and technical barriers like the use of sulfur (input) in laundering. Because of this, the development of a technology for the production of sugar with superior quality, less cost and without sulfur for the laundering would be of great interest for the productive sector. The present work aims to study the process of crystallization of sucrose from sugar solutions of syrup and sugar cane by controlled cooling. A laboratory plant with production capacity of 1 kg of sugar per batch, installed in the laboratory of industrial development of the Sugarcane Technology Center (CTC) in Piracicaba was used for the present work. The results regarding the reduction of impurities initially present in sugar crystals through crystallization by controlled cooling were: 95% in color, 85% in starch and 80% in dextran. For the syrup classified as VVHP, reductions obtained in crystals through crystallization by controlled cooling were: 96% of the final color of the sugar (from 10,100 IU to 361 IU), 98% in the amount of ash conductivity, 84% in the amount of starch and 52% in the amount of dextran. Obtained the results led to the construction of a pilot plant by scaling the process that will be implemented in an industrial unit.
O Brasil, hoje, é o principal produtor e exportador de açúcar do mundo. Foram produzidas na última safra 2008/2009, 31,5 milhões de toneladas de açúcar, das quais cerca de 60% foram exportadas, gerando ao país um domínio de 40% do mercado internacional. No entanto, o açúcar é um produto de relativa dificuldade para comercialização internacional, em razão de fortes restrições, como cotas, subsídios e barreiras técnicas, como a utilização do enxofre (insumo), para o branqueamento. Por isso, o desenvolvimento de uma tecnologia de produção de açúcar de melhor qualidade, com redução de custos e que não necessite de enxofre para o branqueamento seriam de grande interesse para o setor produtivo. O presente trabalho tem por objetivo o estudo do processo de cristalização de sacarose a partir de soluções provenientes de açúcar e xarope de cana-de-açúcar por resfriamento controlado, através de uma planta laboratorial, com capacidade de produção de 1 kg de açúcar por batelada, instalada no laboratório de desenvolvimento industrial do Centro de Tecnologia Canavieira (CTC) em Piracicaba. Os resultados quanto à redução de impurezas presentes inicialmente nos cristais de açúcar através da cristalização por resfriamento controlado foram: de 95% de cor; 85% de amido e 80% de dextrana. Para o xarope classificado como VVHP, as reduções obtidas nos cristais através da cristalização por resfriamento controlado foram: de 96% na cor do açúcar final (de 10.100 UI para 361 UI), de 98% na quantidade de cinzas condutimétricas, de 84% na quantidade de amido e de 52% na quantidade de dextrana. A partir dos resultados obtidos, motivou-se a construção de uma unidade piloto através do scale-up do processo laboratorial, a ser implantada em uma unidade industrial.

Le but de ce travail était d'essayer de comprendre dans quelles mesures les non-sucres présents dans les sirops de sucre ont un effet néfaste sur la cristallisation du saccharose et sur la qualité du sucre obtenu. Pour réaliser cette étude nous avons étudié comparativement différents échantillons industriels de différents origines. Cette étude a nécessité la mise en œuvre d'un certain nombre de techniques de séparation et de fractionnement (ultrafiltration, dialyse, chromatographie d'échange d'ions et d'exclusion stérique. . . ). La combinaison de ces méthodes nous a permis de montrer que l'EP2 danois contient davantage de polyosides de poids moléculaire supérieur à 10000 daltons à caractère non chargés que l'EP2 d'Eppeville. En revanche les fractions moléculaires comprises entre 2000 et 10000 daltons ne semblent pas montrer de différences significatives. On notera que les produits traités industriellement par des résines reminéralisantes et décolorantes ne comportent pratiquement plus de macromolécules. Le relargage à l'alcool des substances colloïdales est un test classique de contrôle, nous avons tenté de l'appliquer aux différents produits sucrés industriels. Nous avons ainsi pu montrer que les non-sucres des EP2 danois sont globalement moins hydrophile que ceux de la sucrerie française qui nous a servi de référence, ce résultat est intéressant car le sucre roux danois obtenu à partir de cet EP2 est de bien meilleure qualité que le sucre roux d'Eppeville. Les macromolécules présentes dans les sirops proviennent en partie de la dégradation des polysaccharides de la betterave qui ont échappé à l'épuration calco-carbonique industrielle, pour comprendre ce phénomène, nous avons montré que la dégradation alcaline des pulpes touche essentiellement les pectines, en revanche hémicelluloses et cellulose résistent bien aux pH basiques. Ce résultat est intéressant pour un approfondissement ultérieur de la connaissance de ces macromolécules. Enfin, dans un but d'application industrielle, nous nous sommes intéressés à l'étude de la valorisation des pulpes de betteraves (décoloration et prévention de l'oxydation des lipides présents) ainsi qu'à l'étude de différentes propriétés fonctionnelles du produit obtenu

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Os mercados dos produtos oriundos da cana-de-açúcar no mundo vêm sofrendo nos últimos anos mudanças estruturais significativas. No cenário brasileiro, houve grande expansão da produção de cana-de-açúcar, impulsionados pela demanda dos carros flex –fuel, além da oportunidade de suprir o volume de açúcar que a União Europeia deixara de colocar no mercado mundial pela eliminação da subvenção aos exportadores de açúcar do bloco. As incertezas dos mercados exigem mudanças de estratégias de negócio, usinas projetadas para produção exclusiva de etanol, alteram sua estratégia para produção conjunta etanol e açúcar. Apesar dos processos comuns para produção de açúcar e etanol, não significa que essa mudança de estratégia seja fácil de ser efetivada, principalmente pelo aspecto energético. Estudos de processo de produção de açúcar mais eficientes energeticamente, com custos menores tem ganhado força na União Europeia, dentre elas a cristalização do açúcar por resfriamento. Vários cenários produtivos inclusive integrados a produção de etanol tem sido desenvolvidos ao longo dos anos. O objetivo do trabalho foi verificar por comparação de cenários, duas tecnologias de cristalização do açúcar (cozimento e resfriamento), em relação ao impacto nos excedentes de energia elétrica quando a produção de açúcar é adicionada a unidades que produzem somente etanol e energia elétrica. Por meio de simulações dos balanços térmicos dos cenários, observou-se uma restrição importante quando adotado a cristalização por cozimento, no que se refere aos volumes de excedentes de energia elétrica, e que pode ser minimizado se adotado o processo de cristalização por resfriamento, podendo assim ser uma alternativa quando se deseja mudar a estratégia do negócio, de produção exclusiva de etanol e energia elétrica para etanol, açúcar e energia elétrica.
Significant structural changes have been occurred in the markets of sugarcane derived products in the world in recent years. Regarding Brazilian scenario, there was a great expansion of sugarcane production due the high demand by flex-fuel cars. In addition the opportunity to meet the volume of sugar that the European Union had failed to put on the world market by eliminating the subvention to sugar exporters in the block. The uncertainties of the markets requires changes in the previus business strategies. Those mills designed for the exclusive production of ethanol, change your strategy to produce both ethanol and sugar. Despite the common processes for the production of sugar and ethanol, it does not mean that this change in strategy is easy to be effected mainly by the energy consumption. New developments in more energy efficient sugar production process, with lower costs have gained strength in the European Union, among them a sugar crystallization by cooling. Many scenarios production and integrated ethanol production have been developed over the past years. The objective of this study was to compare two technologies of sugar production such as boiling and cooling crystallization. The impact on electricity surplus when the production of sugar is added to units that produce only ethanol and electricity is discussed. By simulating the thermal balance of the scenarios, we observed an important restriction adopted when the crystallization by boiling, in terms of electricity surplus amount, which can be minimized by adopting the process of crystallization by cooling. It may therefore be an alternative when a change in the business strategy is desired from an exclusive production of ethanol and electricity to sugar, ethanol and electricity production.

The measurement of the crystal size distribution is a key prerequisite in optimising the growth of sugar crystals in crystalisation pans or for quality control of the final product. Traditionally, crystal size measurements are carried out by inspection or using mechanical sieves. Apart from being time consuming, these techniques can only provide limited quantitative information. For this reason, a more quantitative automatic system is required. In our project, software routines for the automated measurement of crystal size using classical image analysis techniques were developed. A digital imaging technique involves automatically analyzing a captured image of a representative sample of ~ 100 crystals for the automated measurement of crystal size has been developed. The main problem of crystals size measurements using image processing is the lack of an efficient algorithm to identify and separate overlapping and touching crystals which otherwise compromise the accuracy of size measurement. This problem of overlapping and touching crystals was addressed in two ways. First, 5 algorithms which identify and separate overlapping and touching crystals, using mathematical morphology as a tool, were evaluated. The accuracy of the algorithms depends on the technique used to mark every crystal in the image. Secondly, another algorithm which used convexity measures of the crystals based on area and perimeter, to identify and reject overlapping and touching crystals, have been developed. Finally, the two crystal sizing algorithms, the one applies ultimate erosion followed by a distance transformation and the second uses convexity measures to identify overlapping crystals, were compared with well established mechanical sieving technique. Using samples obtained from a sugar refinery, the parameters of interest, including mean aperture (MA) and coefficient of variance (CV), were calculated and compared with those obtained from the sieving method. The imaging technique is faster, more reliable than sieving and can be used to measure the full crystal size distributions of both massecuite and dry product.
Thesis (PhD)-University of KwaZulu-Natal, Durban, 2007.

The main objective of this work is to propose a mechanism for the transfer of impurities into the sucrose crystal. To this end the transfer of impurities into the sucrose crystal was investigated, under crystallisation conditions similar to those found industrially. Most of the impurities, namely, colour bodies, potassium, calcium and starch, were selected on the basis of their industrial importance, but some exotic species, namely lithium and nickel, were chosen to represent other mono- and di-valent ions respectively, and dyes, such as methylene blue, which have been used in work with single crystal sucrose crystallisation, were included to make the results more general. A parameter to measure the rate at which impurities are transferred into the sucrose crystal was proposed. Experiments, carried out in a pilot plant evaporative crystalliser, were performed to establish the effect of selected factors on both the concentrations of impurities found in the sucrose crystal, and on the rate at which these impurities are incorporated into the crystal. All the factors selected, namely the rate of crystallisation, the temperature, the concentration and type of impurity, the diffusivity of the impurity in concentrated sucrose solutions, and the crystal dimensions, are shown to influence the rate of impurity transfer. Only the concentration in the feed and type of impurity, however, affect the final concentration of the impurity in the crystal. Concepts involving partition coefficients and adsorption isotherms were also investigated. The experimental data did not fit the adsorption isotherm models well, but the values obtained for the partition coefficients were similar to those quoted in the literature when exchange types of reactions are operative. Activation energies have been measured, both for the rate of crystallisation of sucrose, and for the rates of impurity transfer. The values obtained, particularly for the rate of impurity transfer, indicate that a transport mechanism is effective. The experimental results have been used to investigate the relevance of two models, one involving a two-step approach and the other an interfacial process, for the incorporation of the impurity into the sucrose crystal. The results obtained indicate that the interfacial breakdown model describes the transfer of all the impurities studied here, except for starch.
Thesis (Ph.D.)-University of Natal, Durban, 1998.

The objective of this work was to determine the operating conditions which would maximise the crystallisation performance of continuous vacuum pans used in the sugar industry. The specific application investigated in detail is crystallisation of high grade product sugar (A-sugar) in a South African raw cane sugar factory. The optimisation studies are based on a detailed dynamic mathematical model of a continuous pan. Whilst this model is based on the published work of others, the selection of variables and the formulation of the equations have been structured to produce a modular model of an individual compartment with the minimum number of independent variables. The independent variables have also been selected to meet the requirements of both a state-space control formulation and those necessary for the dynamic programming technique of optimisation. The modular compartment models are linked together to model a multi-compartment pan and the steady state model is derived as a special case of the dynamic model. For the model to simulate the conditions in South African sugar factories adequately requires appropriate descriptions of sucrose solubility and growth kinetics. Given the limited applicability of published data, experiments were undertaken to determine these parameters. Sucrose solubility in impure solutions was determined in laboratory tests designed to approach equilibrium by dissolution at conditions approximating those during pan boiling. The dependence of crystal growth rate on the concentration of impurity present in the mother liquor was investigated in both laboratory scale and pilot scale batch pan boiling experiments. The primary dependence of crystal growth rate on the super-saturation driving force was determined by fitting the steady state model to results of tests on an industrial scale continuous pan. The dynamic programming technique was used in conjunction with the mathematical model to determine the operating conditions which maximise steady state crystallisation performance. Using the crystallisation parameters determined for South African conditions, this approach has shown that the conventional wisdom of running with high crystal contents in all compartments of continuous pans boiling A-massecuite is not optimum. Pans should operate at lower crystal contents in earlier compartments, only increasing to higher crystal contents towards the final compartment. The specific values depend on seed conditions, pan design and the solubility and growth kinetics. To reap the benefits of being able to determine the optimum steady state operating condition for a continuous pan, it is necessary to be able to achieve effective steady state operation under industrial conditions. This requires both a steady loading on the pan and effective control of the crystallisation conditions within the pan. To stabilise loading, a strategy has been developed which uses buffer tanks in an optimal way to damp out flow fluctuations. This strategy accommodates multiple buffer tanks in series without the amplification of disturbances that occurs with some of the simpler published techniques. The dynamic behaviour of absolute pressure control and compartment feed control were investigated in an industrial scale pan. This work has demonstrated the importance of high quality absolute pressure control and developed techniques for effective automatic tuning of pan feed controls. As part of this research, computer control systems were developed as tools to provide the appropriate monitoring and control of the experiments undertaken.
Thesis (Ph.D.)-University of Natal, 2002.

Crystallization is done in the sugar industry using natural circulation vacuum evaporative crystallizers known as vacuum pans. the fluid which is known as massecuite consists of a suspension of crystals in concentrated molasses. It is highly viscous and slightly non-Newtonian, and laminar conditions prevail in the apparatus. Research on forced convection boiling heat transfer, pressure drop and vapour holdup has been done mostly in turbulent flow under pressures higher than atmospheric, but no studies have been made when boiling viscous fluids under vacuum. This thesis describes a series of experiments which were undertaken with the following objectives: (a) to determine the influence of the pertinent variables on heat transfer, friction losses and vapour holdup while boiling under laminar conditions (b) to produce a method for the calculation of the evaporation and circulation rates in vacuum pans, as this would make possible the optimization of this type of equipment. The apparatus used consisted of a single tube steam heated forced circulation evaporator. The void fraction, pressure and centerline temperature were measured along the tube. The fluids used were syrup, molasses and massecuite covering a thousandfold change in viscosity. The tests were conducted under different conditions of vacuum and steam pressures with varying tube inlet velocities. The experimental results show that the boiling heat transfer coefficient can be correlated as a function of the two phase Reynolds number and dimensionless density ratio and that it is inversely proportional to the tube length to the power of one third. The pressure drop can be estimated using the equation of Oliver and Wright (1964) for bubbly flow. Equations are proposed for calculating the void fraction in the highly subcooled region and point of bubble departure. These equations form the basis of a computer program which by a stepwise and iterative method simulates the boiling process along the tube. Measurements taken on a natural circulation pan with tubes of different length show that this method predicts the effect of the tube length with reasonable accuracy. The limitations of this study are that the experiments were done with a single diameter tube so that the effect of diameter has not been established with certainty. Only sugar products were used in the experiments, and caution is necessary if this method is applied to other fluids.
Thesis (Ph.D.)-University of Natal, Durban, 1985.

N-glycosylation is the most common eukaryotic post-translational modification, impacting on protein stability, folding, and protein-protein interactions. More broadly, N-glycans play biological roles in reaction kinetics modulation, intracellular protein trafficking, and cell-cell communications. The machinery responsible for the initial stages of N-glycan assembly and processing is found on the membrane of the endoplasmic reticulum. Following N-glycan transfer to a nascent glycoprotein, the enzyme Processing α-Glucosidase I (GluI) catalyzes the selective removal of the terminal glucose residue. GluI is a highly substrate-specific enzyme, requiring a minimum glucotriose for catalysis; this glycan is uniquely found in biology in this pathway. The structural basis of the high substrate selectivity and the details of the mechanism of hydrolysis of this reaction have not been characterized. Understanding the structural foundation of this unique relationship forms the major aim of this work. To approach this goal, the S. cerevisiae homolog soluble protein, Cwht1p, was investigated. Cwht1p was expressed and purified in the methyltrophic yeast P. pastoris, improving protein yield to be sufficient for crystallization screens. From Cwht1p crystals, the structure was solved using mercury SAD phasing at a resolution of 2 Å, and two catalytic residues were proposed based upon structural similarity with characterized enzymes. Subsequently, computational methods using a glucotriose ligand were applied to predict the mode of substrate binding. From these results, a proposed model of substrate binding has been formulated, which may be conserved in eukaryotic GluI homologs.