Dissertations / Theses: 'Synthesis of metal phosphates'

1

Lightfoot, P. "Synthesis and characterisation of some transition metal phosphates." Thesis, University of Oxford, 1987. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.382771.

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2

Gaslain, Fabrice O. M. "Synthesis and characterisation of new microporous metal phosphates." Thesis, University of Reading, 2004. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.402611.

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3

Liu, Jun-Yao. "Synthesis and catalytic activity of metal phosphates, phosphites and phosphonates." Thesis, University of Liverpool, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.366368.

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4

Musa, Mazlina. "Ionothermal synthesis of metal aluminophosphates." Thesis, University of St Andrews, 2014. http://hdl.handle.net/10023/4483.

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The aim of this thesis was to synthesise CoAPO-34 and FeAPO-34 using ionothermal synthesis in the presence of organic amines. Using this method provides an alternative route to prepare such materials under low pressure instead of the higher pressure associated with hydrothermal or solvothermal synthesis. Both materials have chabazite (CHA) topology and they are known to act as catalysts. CoAPO-34 was ionothermally prepared using 1-ethyl-3-methylimidazolium bromide (EMIMBr) in presence of 1, 6-hexadiamine (HDA). This study has found that when the synthesis was carried out without HDA, AlPO-11 was preferentially obtained instead of CoAPO-34. Broad line signals which appear between 2000 to 5000 ppm in both spin-echo ³¹P NMR spectra of as-synthesised and calcined CoAPO-34 confirm that the Co²⁺ ions have been successfully incorporated within the framework of the material. FeAPO-34 was synthesised under ionothermal conditions using 1-ethyl-3-methylimidazolium chloride in the presence of ethylenediamine (EDA). In the absence of EDA, the synthesis has produced AlPO-34 instead of FeAPO-34. Broad line signals that appear between 1000 to 14000 ppm in spin-echo ³¹P NMR spectra of both as-synthesised and calcined FeAPO-34 are direct evidence of isomorphous substitution of framework aluminum by Fe(II) or Fe(III). Another aim of this study was to explore the ionothermal synthesis of copper containing aluminophoshate of DNL-1 (Cu/DNL-1). This material was attractive to explore because it contains 20 ring extra-large pores and Cu(I) species in the channels of the framework, potentially giving material the ability to simultaneous store NO and to generate NO from NO₂⁻ anions. Cu/DNL-1 was successfully prepared under ionothermal conditions using EMIMBr and HDA. Without HDA in the synthesis, AlPO-11 was obtained. In this material, copper ions were not incorporated in the Cu/DNL-1 skeleton framework. This was confirmed by absence of broadline signal at >500 ppm in spin-echo ³¹P NMR spectrum of the sample. The copper ions are expected to be present as extra-framework cations. Extra-framework Cu(I) species that were formed by high temperature calcination of Cu/DNL-1 are active to produce NO from NO₂⁻. Therefore, the calcined Cu/DNL-1 can be used to simultaneously store and produce NO from nitrite. This has the potential to signiﬁcantly extend the lifetime of gas delivery in the material to prevent thrombus formation.

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5

Warner, Joanne K. "The synthesis and structural characterisation of some transition metal phosphates." Thesis, University of Oxford, 1992. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.306026.

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6

Burnell, Victoria Anne. "The synthesis, characterisation and ion exchange of mixed metal phosphates." Thesis, University of Birmingham, 2011. http://etheses.bham.ac.uk//id/eprint/3161/.

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This thesis presents work investigating the synthesis and characterisation of a range of mixed metal phosphates. The main aim of the project was to develop materials for the remediation of nuclear waste. In light of this, the materials developed were subject to ion exchange studies and leach testing. The thermal behaviour of the phosphates and nature of the decomposition products were also investigated. This study demonstrates that the true solid solution cannot be formed in any of the mixed metal series investigated, which included zirconium-titanium, germanium-titanium, germanium-zirconium, tin-titanium and tin-zirconium. In all cases a miscibility gap was observed and the reasons for these were established. The co-precipitates that formed were characterised by a variety of analytical techniques which included powder X-ray diffraction (PXRD), thermogravimetric analysis (TGA), pair distribution function (PDF) analysis and X-ray fluorescence (XRF). Structural characterisation was undertaken using both traditional Rietveld analysis of synchrotron X-ray powder diffraction data and PDF analysis of high energy synchrotron total scattering data. The results of the ion exchange studies yielded four exchanged products: strontium exchanged zirconium phosphate, a strontium exchanged zirconium-titanium phosphate and two sodium exchanged titanium phosphate products. Although it was not possible to solve the structures of these phases, they were further characterised by a number of methods and their use as potential stores were investigated by leach testing. The strontium exchanged zirconium phosphate product demonstrated good strontium retention and is recommended for further investigation as a possible strontium waste form.

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7

Eral, Leyla Eanes Mehtap. "Hydrothermal synthesis and characterization of transition metal (Mn and V) oxides containing phosphates/." [s.l.]: [s.n.], 2006. http://library.iyte.edu.tr/tezler/master/kimya/T000562.pdf.

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8

Stark, Michael Andreas [Verfasser]. "Synthesis of nanosized, electrochemically active lithium transition metal phosphates / Michael Andreas Stark." Ulm : Universität Ulm. Fakultät für Naturwissenschaften, 2011. http://d-nb.info/1017543364/34.

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9

Stalder, Sloane Marie. "The synthesis and characterization of some gallophosphates using transition metal complexes as templates." Thesis, Georgia Institute of Technology, 1997. http://hdl.handle.net/1853/27992.

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10

Lu, Ling. "Synthesis and properties of pillared and non-pillared metal organo-phosphates and phosphonates." Thesis, University of Liverpool, 1993. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.385318.

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11

Tuncel, Selcan. "Synthesis Of Iron Borophosphates And Phosphates With Zeo-type Structures." Master's thesis, METU, 2004. http://etd.lib.metu.edu.tr/upload/2/1260460/index.pdf.

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New iron phosphate and borophosphate compounds were synthesized and characterized by single crystal/powder X-ray diffraction, infrared spectroscopy, raman spectroscopy, thermogravimetric analysis, electron microscopy and elemental analysis. Using several compositions, Fey B(PO4)x type of compounds were attempted to be prepared by solid state reactions. The solid state reactions of boron compounds with a phosphating agent has been completed at 950oC. A new product Fe2BP3O12 is synthesized and indexed in this work which is isostructural with Cr2 BP3O12 A single crystal of iron ammonium phosphate, (NH4)3-xHxFeP3O12, was synthesized by a hydrothermal method and characterized. Its X-ray powder diffraction pattern was indexed in orthorhombic system. The unit cell parameters were found to be as a = 7.775 (Å
), b = 7.445(Å
), c = 14.331(Å
) The compound with the formula NH4FeBP2O8OH was synthesized by hydrothermal method. Its X-ray powder diffraction pattern was indexed in monoclinic system. The unit cell parameters were found to be a = 9.336, b = 8.278, c =9.642Å
, and &
#946
= 101.60o, which are good agreement with the literature values. Ferro-axinite type of compound was discovered as single crystals resembling the axinite mineral. The compound was indexed in triclinic system with the unit cell parameters of a = 7.167, b = 8.840 , c = 9.455Å
, &
#945
= 64.83o, &
#946
= 64.83o, &
#947
= 69.42o. A zeotype Fe(H2O)2BP2O8.H2O, which was obtained by hydrothermal methods before, was synthesized by a precipitation method using different initial reactant. In this case, instead of Fe+2, Fe+3 compound was used as a reactant. All the compounds have been investigated by FTIR spectroscopy and the assignments of the functional BO3, BO4 and PO4 groups have been done.

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12

Kruger, John Scott. "Synthesis and characterization of several novel aluminum and gallium phosphates templated by cobalt complexes." Thesis, Georgia Institute of Technology, 1999. http://hdl.handle.net/1853/30553.

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13

Pires, Preciosa de Jesus da Costa. "Synthesis and applications of metal (IV) phosphates, phosphonates and their analogues in oxidation reactions using hydrogen peroxide." Thesis, University of Liverpool, 1995. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.260279.

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14

Menezes, Prashanth W. "New Developments in the Crystal Chemistry of Selected Borophosphates and Phosphates." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2009. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-25105.

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Borophosphates are intermediate compounds of systems MxOy–B2O3–P2O5–(H2O) (M = main group or transition metal) which contain complex anionic structures built of interconnected trigonal–planar BO3 and / or BO4 and PO4 groups and their partially protonated species. The main objective of the present work was to synthesize, characterize and to study the properties of new selected 3d transition metal borophosphates. The selected four elements are scandium (Sc), iron (Fe), cobalt (Co) and nickel (Ni) due to their interesting contributions to borophosphate structural chemistry. The mild hydrothermal method was employed for the syntheses. During the investigation of borophosphates containing alkali–metals and scandium, the following three compounds were prepared and structurally characterized: MISc[BP2O8(OH)] (MI = K, Rb), CsSc[B2P3O11(OH)3] The anionic partial structure of MISc[BP2O8(OH)] (MI = K, Rb) consists of the well known open–branched four–membered rings of alternating borate and phosphate tetrahedra (a loop–branched hexamer with B : P = 1 : 2). The anionic partial structure of CsSc[B2P3O11(OH)3] represents the new type of oligomer containing boron in three– and four– fold coordination (B : P = 2 : 3). This is also the first time that a BO3 group is not only linked to borate species but also to a phosphate tetrahedron. This kind of oligomer was already predicted for borates but was never observed. By this, CsSc[B2P3O11(OH)3] is a special compound with regard to the structural building principles of borates and borophosphates. The significant differences in the crystal structures of MISc[BP2O8(OH)] (MI = K, Rb) and CsSc[B2P3O11(OH)3] may be due to the higher coordination number of cesium. Thermal treatment (up to 1000 ºC) of these compounds resulted in white crystalline products containing new phases with unknown crystal structures. Besides the discovery of alkali–metal scandium borophosphates, five new alkali metal scandium hydrogenphosphates were synthesized and structurally characterized: Li2Sc[(PO4)(HPO4)], MISc(HPO4)2 (MI = K, Rb, Cs, NH4) It was already predicted that open framework scandium phosphates should be isotypes of the respective indium phosphates. It was also stated that there should be a whole family of scandium hydrogenphosphates as we were able to confirm with the five novel compounds. Our systematic study reveals the structural changes of the anionic partial frameworks with increasing ionic radii of the alkali–metal ion. With respect to the M―T connections (M = six coordinated central metal atom, T = four coordinated phosphorous atom) the channel size increases from 8–membered rings in Li2Sc[(PO4)(HPO4)] to 12–membered rings in MISc(HPO4)2 (MI = K, Rb, Cs, NH4). KSc(HPO4)2 exhibits a new structure type in the family of monohydrogenphosphates with the general formula MIMIII(HPO4)2. This provides further evidence that scandium is a suitable element for the synthesis of framework structures with different channel sizes. The observation that in analogy to MISc(HPO4)2 (MI = Rb, Cs, NH4) a compound exists where the MI site is replaced by H3O+ gives rise to the hope that ion exchange properties could be of interest in this class of compounds. In addition, the possible existence of further modifications (as reported for the element–combinations RbV, NH4V, RbFe, and CsIn) shoud be investigated by thermoanalytical and X–ray methods. The extensive studies on borophosphate containing the transition metals Fe, Co, Ni together with alkaline earth–metals (Mg, Ca, Sr, Ba) led to the preparation of 13 compounds containing the combination of two different divalent M1IIM2II ions: CaM2II[BP2O7(OH)3] (M2II = Fe, Ni), BaM2II[BP2O8(OH)] (M2II = Fe, Co), SrFe[BP2O8(OH)2], CaCo(H2O)[BP2O8(OH)]•H2O, M1II0.5M2II(H2O)2[BP2O8]•H2O (M1II0.5 = Ca, Sr, Ba; M2II = Fe, Co, Ni) The anionic partial structure of CaM2II[BP2O7(OH)3] (M2II = Fe, Ni) consists of a tetrahedral triple [BP2O7(OH)3]4-, built from a central (HO)2BO2 tetrahedron sharing common vertices with two (H0.5)OPO3 tetrahedra. The complex anions in the crystal structure of BaM2II[BP2O8(OH)] (M2II = Fe, Co) comprises open–branched four–membered rings, [B2P4O16(OH)2]8-, which are formed by alternating (HO)BO3 and PO4 tetrahedra sharing common corners with two additional PO4 branches. The interconnection of these complex anions with M2II coordination octahedra (M2II = Fe, Co, Ni) by sharing common corners results in overall three–dimensional frameworks which contain channels filled with the M1II ions (M1II = Ca, Ba). The anionic partial structure of SrFe[BP2O8(OH)2] is built from a central (HO)2BO2 tetrahedron sharing common vertices with two PO4 tetrahedra. Surprisingly, SrFe[BP2O8(OH)2] represents the first example in the structural chemistry of borophosphates where the charge of the anionic partial structure is balanced by a divalent and a trivalent species (MIIMIII). Although being a member of the M1IIM2II[BP2O8(OH)] family the crystal structure of CaCo(H2O)[BP2O8(OH)]•H2O is different. Interestingly, this is the first case in the borophosphate structural chemistry where dimers of cobalt coordination octahedra together with borophosphate oligomers form a (two–dimensional) layered structure. The helical borophosphates M1II0.5M2II(H2O)2[BP2O8]•H2O (M1II0.5 = Ca, Sr, Ba; M2II = Fe, Co, Ni) contain one–dimensional infinite loop–branched borophosphate helices built of alternatively distorted borate and phosphate tetrahedra. Up to now, the group of compounds with 1[BP2O8]3– helical chain anions has been synthesized only in combination with different cations MIMII and MIII (MI = Li, Na, K; MII = Mg, Mn, Fe, Co, Ni, Zn; MIII = Sc, In, Fe). The systematic investigation on helical borophosphates of transition metals (Fe, Co, Ni) and alkaline–earth metals showed that it is also possible to accommodate divalent metal cations within the structure without disturbing the anionic partial structure. It was not possible to find the completely ordered structural model for the compounds M1II0.5M2II(H2O)2[BP2O8]•H2O (M1II0.5 = Ca, Sr, Ba; M2II = Co) but the substructure presented shows good agreement with the ordered known helical borophosphate compounds. Interestingly, it was also possible to judge the “kind of superstructure” against the crystal morphology. Syntheses of one of the few examples of borophosphates containing layered anionic partial structures (63 net topology) containing transition metal cations (Fe, Co, Ni) was realized with 6 isotypic compounds: MII(H2O)2[B2P2O8(OH)2]•H2O (MII = Fe, Co, Ni, Ni0.5Co0.5, Ni0.8Zn0.2, Ni0.5Mg0.5) The compounds MII(H2O)2[B2P2O8(OH)2]•H2O (MII = Fe, Co, Ni) adopt the structure type of Mg(H2O)2[B2P2O8(OH)2]•H2O characterized by a two–dimensional borophosphate anion. Substitution on the transition metal sites was shown to be possible (Ni0.5Co0.5) realized for this structure type. With the synthesis of Ni0.8Zn0.2(H2O)2[B2P2O8(OH)2]•H2O and Ni0.5Mg0.5(H2O)2[B2P2O8(OH)2]•H2O it was also proved that magnetically diluted samples can be prepared in analogy to Mg1–x Cox(H2O)2[B2P2O8(OH)2]•H2O (x = 0.25). The thermal stability of these compounds is very similar with a slight shift to higher decomposition temperatures for the Ni0.5Mg0.5(H2O)2[B2P2O8(OH)2]•H2O. In contrast to other borophosphates such as MIMII(H2O)2[BP2O8]∙H2O and MIII(H2O)2[BP2O8]∙H2O, it is not possible to rehydrate partially dehydrated samples even though the crystal structure may suggest this property. This shows that the aqua–ligands significantly contribute to the stability of the structure. The magnetic behavior of MII(H2O)2[B2P2O8(OH)2]•H2O (MII = Fe, Ni) corresponds well with separated 3d ions without strong magnetic interactions down to 1.8 K. Quite surprising was the remarkable change in the crystal habit that was observed during the synthesis upon addition of alkali–metal cations. Syntheses with the absence of alkali–metals lead to a change in the crystal habit by reducing of the number of faces in direction of the more simple prismatic morphology. Our research on borophosphates containing mixed transition metals led to the preparation of a borophosphate and a phosphate: FeCo(H2O)[BP3O9(OH)4], Fe1.3Co0.7[P2O7]∙2H2O The anionic partial structure of FeCo(H2O)[BP3O9(OH)4] is an open–branched tetramer built from (HO)BO3 sharing common O–corners with one (HO)PO3, one (HO)2PO2 and one PO4 group. The crystal structure is an isotype to Mg2(H2O)[BP3O9(OH)4]. Fe1.3Co0.7[P2O7]∙2H2O contains the diphosphate composed of two corner–sharing tetrahedra (isotypic to MII[X2O7]∙2H2O (MII = Mg, Mn, Co, Fe and X = P, As). However, the crystal structure of both, FeCo(H2O)[BP3O9(OH)4] and Fe1.3Co0.7[P2O7]∙2H2O, contains octahedral zigzag chains, which are interconnected by the respective tetrahedral anions. The octahedral chains in these crystal structures are closely related to the octahedral arrangements in MIIH2P2O7 (MII = Co, Ni) which exhibit a field-induced metamagnetic behavior from an antiferromagnetic state to a ferromagnetic state and to MII[BPO4(OH)2] (MII = Mn, Fe, Co) which indicate a low-dimensional antiferromagnetic correlation of the MII ions by dominant exchange interactions within the one–dimensional octahedral chain structure. Therefore, due to the similar structural features, FeCo(H2O)[BP3O9(OH)4] and Fe1.3Co0.7[P2O7]∙2H2O may exhibit interesting magnetic properties. Thermal investigation revealed that both compounds are stable until 300 ºC and transform into pyrophosphates at higher temperatures. Fe1.3Co0.7[P2O7]∙2H2O represents the first hydrated mixed divalent cation diphosphate.

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15

Abu-Shandi, Khalid Hamad. "Metal phosphates from syntheses and structures to applications in sorption, catalysis and teeth erosion protection /." [S.l.] : [s.n.], 2003. http://www.freidok.uni-freiburg.de/volltexte/691.

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16

Xu, Chunbao. "Continuous and batch hydrothermal synthesis of metal oxide nanoparticles and metal oxide-activated carbon nanocomposites." Diss., Available online, Georgia Institute of Technology, 2006, 2006. http://etd.gatech.edu/theses/available/etd-07302006-231517/.

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Thesis (Ph. D.)--Chemical and Biomolecular Engineering, Georgia Institute of Technology, 2007.
Teja, Amyn, Committee Chair ; Kohl, Paul, Committee Member ; Liu, Meilin, Committee Member ; Nair,Sankar, Committee Member ; Rousseau, Ronald, Committee Member.

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17

Anantharaman, Ganapathi. "Synthesis and structural studies of group 12 metallasiloxane and phosphonate aggregates precursors for metal silicate and phosphate assemblies /." [S.l.] : [s.n.], 2003. http://deposit.ddb.de/cgi-bin/dokserv?idn=97033754X.

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Abu-Shandi, Khalid. "Metal phosphates: From syntheses and structures to applications in sorption, catalysis and teeth erosion protection from syntheses and structures to applications in sorption, catalysis and teeth erosion protection /." [S.l. : s.n.], 2003. http://www.bsz-bw.de/cgi-bin/xvms.cgi?SWB10547312.

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19

Oyetola, Samuel. "Synthese et etude des composes a**(i)m**(v)p::(2)o::(8) (a = k, rb, cs; m = sb, nb, mo, ta) et des acides echangeurs ioniques hm**(v)(po::(4))::(2),xh::(2)o (m = sb, ta), nouveaux types de luminophores potentiels : les phases (m'**(iii)::(1/2)m**(v)::(1/2))p::(2)o::(7) (m'=sb, bi, ln; m=sb, nb, ta)." Nantes, 1988. http://www.theses.fr/1988NANT2008.

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Premilere partie: la plupart des phases du titre ont une structure en couches voisine de celle de zrp-alpha. Le traitement en milieu acide des phases en couches km**(i)(po::(4))::(2), m=sb, ta permet d'obtenir les acides correspondant hm**(v)(po::(4))::(2)xh::(2)o. Un autre acide, hta(po::(4))::(2) 3d, peut etre obtenu directement par voie seche, description de sa structure tridimensionnelle. Determination de la teneur en eau, de la structure et du comportement thermique de ces differents acides dont la thermolyse conduit a des phases originales qui sont etudiees. Seconde partie: dans la premiere famille, les phases (m'**(iii)::(1/2)m**(v)::(3/2)) (po::(4))::(3) sont de type nasicon ou sc::(2)(no::(4))::(3) ou d'un nouveau type structural, dans la seconde, les phases m'**(iii)::(1/2)m**(v)::(1/2))p::(2)o::(7) presentent des structures voisines de celle de zrp::(2)o::(7)

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20

Ahmed, Aliya. "Structural studies of mixed metal phosphates." Thesis, Queen Mary, University of London, 2001. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.272125.

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Saunders, Alex Michael. "Synthesis of deuterated phosphatidylinositol phosphates." Thesis, University of Oxford, 2017. https://ora.ox.ac.uk/objects/uuid:65f93fcc-791a-491f-88c5-8ccb5db58592.

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Phosphatidylinositol phosphates (PtdInsPn) are intracellular signalling molecules that are important in many key biological processes, in particular Ca2+ signalling pathways. Dysfunction of these processes has been implicated in numerous diseases including diabetes and many cancers. Some aspects of PtdInsPn signalling have been heavily investigated; PTEN, PKC/Akt, PtdIns3K and PtdIns4K are all important therapeutic targets that have seen much attention in industrial endeavours. Inositol-based probes and tool compounds for these targets typically incorporate a fluorescent tag or photo-crosslinking group, usually at the lipid tails. It is increasingly apparent that the nature of the lipid chains plays a key role in determining the sub-cellular localisation of the PtdInsPn and hence modification of the lipids is potentially detrimental to the biological function of the tool compounds. An additional challenge in the development of inositol-based tools compounds is the difficult and lengthy syntheses that are employed to obtain the target compounds. To address this, we have developed a novel asymmetric route that allows rapid synthesis of PtdIns and PtdIns(4,5)P2. This route has been designed to allow incorporation of multiple deuterium atoms onto the myo-inositol ring (C-perdeuterated). To achieve this, we began with the aromatic compound quinol and built up the myo-inositol ring piecewise, allowing for deuterium incorporation. This methodology utilised a Pd-catalysed dynamic kinetic resolution on a conduritol B derivative to form optically-pure myo-inositol derivatives in high e.e. ( > 99%) toward the synthesis of D6-PtdIns(4,5)P2. The incorporation of deuterium into these compounds should be minimally disruptive to their biological activity, while the difference in molecular mass between the endogenous and tool compounds enables their use in a range of biological assays. In addition, the incorporation of the deuterium onto the myo-inositol ring will allow for the detection of downstream effects relating to the myo-inositol ring post-hydrolysis of PtdIns(4,5)P2 to be observed, which is currently not possible with other probes.

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22

Stock, Joseph R. "Synthesis of BIS(2.2,2-Trifluoroethyl) vinylphosphates." Connect to online version at OhioLINK ETD Connect to online version at Digital.Maag, 1998. http://hdl.handle.net/1989/4785.

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Hodson, Lisa Francesca. "Catalysis by single and mixed metal phosphates." Thesis, University of Liverpool, 1996. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.337133.

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Ewald, Bastian. "Borophosphate der Haupt- und Nebengruppenmetalle: Synthese, Charakterisierung und Strukturchemische Klassifizierung." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2006. http://nbn-resolving.de/urn:nbn:de:swb:14-1165332117390-21543.

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Es werden neue Erkenntnisse über Borphosphat und Borophosphate der Haupt- und Nebengruppenmetalle vorgestellt. Neben Hydrothermalsynthesen und Feststoffreationen, die üblicherweise zur Synthese von Borophosphaten angewendet werden, haben insbesondere die solvothermalen Experimente mit Alkoholen bzw. Alkohol-Wasser-Mischungen zu neuen Ergebnissen geführt. Es wurden neue Borophosphate und Borat-Phosphate in den Systemen MxOy–B2O3–P2O5(–H2O) (M = K+, Rb+, Mg2+, Sc3+, Pr3+, Sm3+, In3+) dargestellt, weitere Verbindungen enthalten neben Mg2+ weitere Kationen der Haupt- und Nebengruppenmetalle (Ca, Sr, Ba, Mn, Fe, Co, Zn). Darüberhinaus gelang die Darstellung bislang unbekannter Scandium- und Lanthanphosphate(III) sowie von sauren Alkalimetall-Scandiumphosphaten(V). Aus Synthesen in Gegenwart von Ethylendiamin und Diazabizyklooktan wurden ferner zwei neue templatierte Scandiumphosphate mit porösen Gerüststrukturen erhalten. Die Kristallstrukturen aller Verbindungem wurden rötgenographisch anhand von Einkristallaufnahmen oder Pulverdaten aufgeklärt. Die Charakterisierung der Präparate erfolgte mit Röntgenpulverdiffraktometrie, EDX- und Elementaranalysen sowie durch Schwingungsspektroskopie und thermische Stabilitätsuntersuchungen. Zur Klassifizierung von (Metallo)borophosphaten wird eine Struktursystematik vorgeschlagen, welche Borophosphate und Metalloborophosphate entsprechend ihrer anionischen Teilstrukturen hierarchisch klassifiziert und in Analogie zur Terminologie der Silikate (nach Liebau) beschreibt. In Anlehnung an bestehende Konzepte für Boratminerale geht das Klassifizierungsschema dabei von einfachen Oligomeren aus. In einer struktursystematischen Übersicht wurden alle bis dato bekannten (Metallo)Borophosphate hierarchisch klassifiziert und sind in einer Übersicht vorgestellt. Beobachtete Verknüpfungsregeln und der Einfluss der Zusammensetzung B:P auf die Dimensionalität und die Verknüpfungsmuster der anionischen Teilstruktur werden diskutiert.

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25

Jakeman, R. J. B. "Structural studies on metal phosphates and related compounds." Thesis, University of Oxford, 1986. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.375264.

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26

Raguž, Branimir [Verfasser]. "Synthese und Charakterisierung von Lithium-metall(I)-phosphaten / Branimir Raguž." Bonn : Universitäts- und Landesbibliothek Bonn, 2020. http://d-nb.info/1224270630/34.

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27

Seo, Jin Seog. "Hydrolyzing phosphates with metal ions : di and trinuclear approach." Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1997. http://www.collectionscanada.ca/obj/s4/f2/dsk3/ftp04/nq30381.pdf.

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28

Liang, Tao. "Chiral Phosphoric Acids and Alkaline Earth Metal Phosphates Chemistry." Thesis, University of South Florida, 2014. http://pqdtopen.proquest.com/#viewpdf?dispub=3632228.

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Asymmetric synthesis and catalysis is one of the leading research areas in chemistry society, for its versatility and efficiency in obtaining chiral molecules that found the vast majority in natural active compounds and synthetic drugs. Developing asymmetric catalytic methodology is at the frontier in both industrial and academic research laboratories. Enantioselective organocatalysis has emerged as a powerful synthetic tool that is complementary to metal-catalyzed transformations. The development of chiral phosphoric acid and metal phosphate as catalysts has been a breakthrough in recent years. Chiral phosphoric acids have been shown to be powerful catalysts in many organic transformations. Moreover, chiral metal phosphates, which formed by simply replacing the proton in phosphoric acid with metals, have introduced new catalytic activations and broaden the scope of phosphoric acids. This thesis details new highly enantioselective chiral phosphoric acid-catalyzed Pinacol rearrangement and robust alkaline phosphates catalytic system, which utilizes novel carbonyl activation.

The Pinacol rearrangement has long been known to be difficult to control in terms of regioselectivity and stereoselectivity. The initial studies found that indolyl-diol compounds can be treated with chiral phosphoric acids to afford the Pinacol rearrangement with high regio- and enantioselectivity. Over 16 chiral phosphoric acids were screened, and it was found an H8-BINOL-phosphoric acid variant with 1-naphthyl groups at 3 and 3' position was the excellent catalyst. This asymmetric transformation is tolerant toward variety of substituents both on the indole ring and migrating groups.

During the study, it was found that different ways to generate the catalyst had critical effect on this catalytic transformation. Only those phosphoric acids washed with HCl after column chromatography afforded the rearrangement products with high enantioselectivity. And those without treating with HCl were found contaminated by alkaline metals. These "contamination" catalysts were also found active with carbonyl activations.

A highly enantioselective catalytic hetero-Diels-Alder reaction of alpha-keto esters has been developed with chiral alkaline metal phosphates. A calcium 1-naphthyl-BINOL phosphate was found to be the optimum catalyst. A large range of alpha-keto esters as well as isatins can be applied in this alkaline phosphates catalytic system with high efficiency and selectivity. The structure of the catalyst is detailed for the first time by X-ray crystal structure analysis. A proposed Transition state model is provided based on the catalyst crystal structure and Raman spectroscopy analysis.

This methodology was further developed with an asymmetric Mukaiyama-Michael addition of beta,gamma-unsaturated alpha-keto ester. The best catalyst was found to be a magnesium chiral phosphate. And the transformation was found capable of tolerating a wide variety of beta,gamma-unsaturated alpha-keto esters.

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Spencer, Peter C. "Synthesis and reactions of protected aminoacyl ethyl phosphates." Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1998. http://www.collectionscanada.ca/obj/s4/f2/dsk1/tape10/PQDD_0007/MQ40736.pdf.

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30

Checker, N. J. "The synthesis and properties of novel condensed phosphates." Thesis, University of Birmingham, 2006. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.502587.

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31

Whyte, Gillian. "Synthesis and evaluation of receptors for phosphatidylinositol phosphates." Thesis, Imperial College London, 2013. http://hdl.handle.net/10044/1/18967.

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Phosphatidylinositol phosphates (PIPs) are signalling phospholipids with a diverse set of cellular functions. The most important of these PIPs are phosphatidylinositol (4,5) bisphosphate (PI(4,5)P2) and phosphatidylinositol (3,4,5) trisphosphate (PI(3,4,5)P3). These two are responsible for a number of cellular events which regulate cell growth, proliferation and apoptosis. Deregulation of PIP levels disrupts these pathways and can therefore lead to uncontrolled cell growth and which can lead to tumourigenesis. Control of PIP levels has been identified as a potential target for diagnosis and intervention in diseases including Alzheimer’s disease, cancer, and the genetic disorder Lowe Syndrome. The use of small molecules that bind PIPs has been shown by our group to interfere with protein-PIP interactions. By preventing proteins from binding to PIPs, the effective concentration of the target PIP is reduced, proteins are not recruited to the membrane for activation and downstream signalling pathways are attenuated. Therefore, in this project a series of small artificial receptors were synthesised and were shown to bind PI(4,5)P2 and PI(3,4,5)P3. The aim of this was to control their effective levels and manipulate their downstream signalling pathways. PI(4,5)P2-binding receptors were developed based on existing lead compounds established within our group. Comparison of a receptor with only one binding motif with the established two motif receptor showed differences in affinity as well as specificity for the phospholipid target PI(4,5)P2 over the headgroup IP3. In cells, the effect of the receptors on the downstream signalling pathways was examined using phosphorylated Akt as an indicator of this pathway’s activation. Two fluorescent receptors were designed and one of these was used as a novel PI(4,5)P2 detection tool on immobilised phospholipid. Preliminary results show that this receptor may also be used to directly image PI(4,5)P2 in fixed cells. Novel PI(3,4,5)P3 receptors were designed with phosphate-binding motifs and a range of spacers. The specificity of each receptor was identified and binding affinities towards PI(3,4,5)P3 were established. Inhibition of protein-lipid interaction and inhibition of PIP-metabolising enzymes were also studied. The effect of these new receptors in attenuating the Akt pathway in cancer cells was also investigated, and they were found to lack the efficacy of PI(4,5)P2-binding receptors. The ability of some of these artificial receptors to bind phospholipids in the cell and affect subsequent signalling pathways indicates that phospholipids are a viable additional drug targets for many diseases.

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Wang, Meng Fang. "The synthesis of carbohydrate analogues of inositol phosphates." Thesis, University of Newcastle Upon Tyne, 1992. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.386707.

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33

Torres-Trevino, G. "Synthesis and characterisation of new lithium zinc phosphates." Thesis, University of Aberdeen, 1986. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.372443.

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34

Cooke, Allan Melvin. "Synthesis and biology of inositol phosphates and thiophosphates." Thesis, University of Leicester, 1991. http://hdl.handle.net/2381/34061.

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35

Rajamanickam, Muralikrishnan. "The asymmetric synthesis of enol phosphates and their application in total synthesis." Thesis, University of Strathclyde, 2015. http://oleg.lib.strath.ac.uk:80/R/?func=dbin-jump-full&object_id=27005.

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The synthesis of a wide range of highly valuable enol phosphate products has been carried out. The use of carbon centred magnesium bases, previously developed in the group has allowed the formation of kinetic enol phosphate products under room temperature conditions. By applying specific quench conditions such as the reverse addition quench condition yields up to 95% were obtained while using di-tertbutylmagnesium base. Interestingly acetophenone derivatives required the use of di-mesitylmagnesium base to access the corresponding enol phosphate compounds. Such enol phosphates can also be obtained under an enantioenriched fashion with the use of chiral magnesium bisamide bases. Previously studied C2- and pseudo C2-symmetric magnesium amide bases were synthesised and the process optimised to obtain up to 95% yield and 95:5 of selectivity on the benchmark substrate. A novel co-addition quench protocol was developed to access high reactivity and selectivity at mild temperature conditions (-20 °C).The high stability of enol phosphate products allowed a detailed study of the chiral magnesium amide bases. Such study allowed the development of a practical methodology towards chiral alkyl-magnesium amide bases allowing similar results to chiral magnesium bisamide bases with half the amount of chiral amine. Further investigations of the reactive species in solution through DOSY NMR techniques were also carried out. Finally the sum of knowledge gained through synthesis and application of enolphosphates allowed the total synthesis of a natural product (+)-Sporochnol. The key transformation of the synthesis consisted on the desymmetrisation of a prochiral ketone to generate an enantioenriched enol phosphate followed by a Kumada cross coupling reaction. The novel Kumada coupling reaction was initially developed for the synthesis of (+)-Sporochnol. With the success encountered in such methodology we further developed the reaction, which, ultimately allowed the cross coupling of unactivatedenol phosphate compounds with alkyl Grignard reagents at room temperature using commerically available and air stable PEPPSI catalysts.

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36

Franklin, Ilona Louise. "Studies of metal substituted alumino-phosphates and other related systems." Thesis, University College London (University of London), 2005. http://discovery.ucl.ac.uk/1445536/.

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The research within this thesis has concentrated around the identification and catalytic understanding of the acid and redox properties of a series of metal substituted aluminophosphates, silicoaluminophosphates and polyoxometalates. The aim being to understand how the active metal sites were co-ordinated, to what degree of substitution had been successfully achieved and finally the direct relation this information had in understanding the degree of reaction for the various catalytic processes. In most part hydrothermal synthesis was employed, the exception being in the case of the polyoxometalate and polyoxometalate layered double hydroxide synthesis. Characterisation was achieved through the use of many analytical techniques predominantly X-ray diffraction (XRD) and extended X-ray spectroscopy (XAS). In total, four commercially important reactions were studied. Firstly, the shape selective and redox properties associated with (a) the substitution of different metal ions within the same aluminophosphate framework and (b) the substitution of the same metal ion within different aluminophosphate frameworks were characterised and investigated for the methanol to olefin (MTO) reaction to demonstrate the activity and selectivity of different frameworks in the production of a range of olefins. Secondly, several transition metal ion-exchanged zeolites and aluminophosphates were synthesised, characterised and subsequently analysed for the hydroxylation of phenol. Here temperature effects were also investigated to see what, if any effect it had upon the final conversion of phenol. Thirdly, a series of bifunctional platinum impregnated silicoaluminophosphate (Pt/SAPO) and metal substituted aluminophosphate (Pt/MeAlPO) catalysts were synthesised, characterised then investigated to understand how their acidic nature effected the catalytic activity and selectivity for the hydroisomerisation of n-heptane. Finally, the properties of several cobalt-substituted polyoxometalates (POM's) and polyoxometalate pillared layered double hydroxides (POM-LDH's) were studied and investigated for their catalytic activity for the oxidation of cyclohexane with molecular oxygen in the presence of TBHP.

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37

Ciszewski, Gregory M. "Synthesis of Bis(2,2,2-trifluoroethyl) Phosphonates A New Model for the Synthesis of Phosphonates." Connect to online version at OhioLINK ETD Connect to online version at Digiatl.Maag, 1998. http://hdl.handle.net/1989/4786.

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38

Battaggia, S. "Approaches toward the synthesis of oligonucleotide 2'0,3'0-cyclic phosphates." Thesis, Queen's University Belfast, 2003. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.273172.

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39

Riley, Andrew M. "Inositol phosphates and analogues : synthesis, stereochemistry and molecular recognition." Thesis, University of Bath, 1996. https://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.484225.

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40

Spiers, Ian D. "Synthesis, crystallography and biological activity of myo-inositol phosphates." Thesis, Aston University, 1996. http://publications.aston.ac.uk/11047/.

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The antioxidant property of myo-inositol hexakisphosphate is important in the prevention of hydroxyl radical formation which may allow it to act as a 'safe' carrier of iron within the cell. Here, the hypothesis that the recently discovered natural product, myo-inositol 1,2,3-trisphosphate represents the simplest structure to mimic phytate's antioxidant activity has been tested. The first synthesis of myo-inositol 1,2,3-trisphosphate has been completed, along with its X-ray structure determination and that of key synthetic intermediates. Iron binding studies of myo-inositol 1,2,3-trisphosphate demonstrated that phosphate groups with the equatorial-axial-equatorial conformation are required for complete inhibition of hydroxyl radical formation. myo-Inositol monophosphatase is a key enzyme in recycling myo-inositol from its monophosphates in the brain and its inhibition is implicated in lithium's antimanic properties. Current synthetic strategies require inositol compounds to be protected (often with more than one group), resolved, phosphorylated and deprotected to produce the desired optically active myo-inositol phosphates. Here, the synthesis of myo-inositol 3-phosphate has been achieved in only 4 steps from myo-inositol. The stereoselective addition of the chiral phosphorylating agent (2R,4S,5R)-2-chloro-3,4-dimethyl-5-phenyl-1,3,2-oxazaphospholidin-2-one to a protected inositol intermediate allowed separation of diastereoisomers and easy deprotection to myo-inositol 3-phosphate. This strategy also allows the possible introduction of labels of oxygen and sulphur to give a thiophosphate of known stereochemistry at phosphorus which would be useful for the analysis of the stereochemical course of phosphate hydrolysis catalysed by inositol monophosphatase.

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41

Doolittle, John William. "Synthesis of microporous faujasitic zincophosphates in novel environments." Connect to resource, 2005. http://rave.ohiolink.edu/etdc/view?acc%5Fnum=osu1116983708.

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Thesis (Ph.D.)--Ohio State University, 2005.
Title from first page of PDF file. Document formatted into pages; contains xxiii, 248 p.; also includes graphics. Includes bibliographical references (p. 226-248). Available online via OhioLINK's ETD Center

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42

Keita, Ousainou Ansumana. "The synthesis of new phenylhydroxyiodonium phosphates from (diacetoxyiodobenzene) and dialkyl phosphates and their use in the α-phosphorylation of ketones to mono-ketol phosphates." University of Akron / OhioLINK, 2008. http://rave.ohiolink.edu/etdc/view?acc_num=akron1197558427.

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43

Nose, Masafumi. "Studies on Sodium-containing Transition Metal Phosphates for Sodium-ion Batteries." 京都大学 (Kyoto University), 2016. http://hdl.handle.net/2433/215565.

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44

Woinaroschy, Kristina Michaela. "Cyclen transition metal complexes as biomimetic catalysts, phosphate anion sensors and building-blocks in supramolecular assemblies." kostenfrei, 2007. http://www.opus-bayern.de/uni-regensburg/volltexte/2009/890/.

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45

Noble, Nicholas Jason. "Synthesis of novel phosphorothioate and pyrophosphate analysis of inositol phosphates." Thesis, University of Leicester, 1992. http://hdl.handle.net/2381/33831.

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A novel synthesis of cyclic pyrophosphates was developed. The vicinal bisphosphorothioate, l-phenyl-ethane-l,2-bisphosphorothioate, was synthesised using phosphorus (III) chemistry. This model compound was used to investigate the formation of the cyclic 7-membered pyrophosphate; N-bromosuccinimide was found to be the reagent of choice, giving the cyclic pyrophosphate in moderate yield. Activation of the bisphosphorothioate moiety by S-methylation, increased the yield of the pyrophosphate, as id reducing the conformational mobility of the vicinal bisphosphorothioate. Isotopic labelling experiments were used to investigate the mechanism of the reaction. However, it was concluded that the reaction proceeded via a complex combination of reaction pathways. The synthesis of the bacterial metabolite cyclic-2,3-bisphosphoglycerate was attempted using the new method, unfortunately, cyclic-2,3-bisphosphoglycerate was not isolated. In order to prepare pyrophosphate analogues of myo-inositol-1,4,5-trisphosphate, it was necessary to prepare compounds such as myo-Inositol-1-phosphate-4,5- bisphosphorothioate and 6-deoxy-D-myo-inositol-l,4,5-trisphosphorothioate. Inositol-l,4-bisphosphate-5-phosphorothioate was synthesised from a precursor, the structure of which was determined by 2-dimensional NMR spectroscopy. myo-Inositol- 1-phosphate-4,5-bisphosphorothioate and myo-inositol-1,4-bisphosphate-5- phosphorothioate were found to be potent inhibitors of the inositol-5-phosphatase enzyme, whereas 6-deoxy-D-wyo-inositol-l,4,5-trisphosphorothioate was found to be a weak inhibitor of the inositol-5-phosphatase enzyme. Initially, the synthesis of an inositol pyrophosphate was attempted where phosphate scrambling, a potential side reaction, could not compete with the formation of the pyrophosphate. To this end, the desulphurisation of 6-deoxy-2,3-cyclohexylidene-D- myo-inositol-l,4,5-trisphosphorothioate was attempted. The reaction gave the 6-deoxy- 2,3-cyclohexylidene-D-myo-inositol-l-phosphate-4,5-pyrophosphate in good yield. myo-Inositol-1-phosphate-4,5-bisphosphorothioate was prepared from wyo-inositol and was treated with N-bromosuccinimide. The result of the reaction was to give the target molecule myo-inositol-1-phosphate-4,5-pyrophosphate again in high yield. Unfortunately, the pyrophosphate was found not to be active at releasing Ca2+ nor active towards the phosphoinositide cycle enzymes.

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46

Carkner, Andrew. "Green metal nanoparticle synthesis." Thesis, McGill University, 2008. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=22037.

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Title: Green Metal Nanoparticle Synthesis Silver and nickel nanoparticles have diverse applications in catalysis, composite materials, and electronics. Current production methods rely on high-energy processes or harsh chemicals; thus it is preferable to use environmentally benign compounds for their synthesis. This project studied the aqueous synthesis of nickel nanoparticles from nickel acetate using glucose, formate, and hydrazine as reducing agents. It was found that although the reactions are thermodynamically favourable, nickel nanoparticles could not be produced using glucose or formate at pH 4-12 and T ≤ 100oC. The conversion was negligible even after 8 hours. With hydrazine, high temperature and pH are necessary for a rapid reaction. At pH 12, 100oC, and 20 mM nickel acetate, a conversion of 70% can be achieved in 30 minutes. For pH below 10 or temperature below 80oC, conversion is negligible even after 3 hours.
Titre: Production vert de nanoparticules métalliques Les nanoparticules d'argent et de nickel ont de diverses applications en catalyse, matériaux composites et électronique. Cependant la production actuelle utilise soit beaucoup d'énergie soit de composés dangereux ; il sera mieux pour la santé et l'environnement de trouver d'alternatives. Ce projet a examiné le glucose et le formate comme alternatifs au hydrazine pour la synthèse aqueuse des nanoparticules. Quoique les conditions thermodynamiques sont favorables, je n'ai pas pu produire de nanoparticules de nickel sauf avec le hydrazine dans la région pH 4-12 et T ≤ 100oC. Avec le glucose ou le formate, la conversion demeure insignifiant après 8h. Avec le hydrazine, une haute température et pH sont nécessaires pour une réaction rapide. Avec pH 12, 100oC et 20 mM d'acetate de nickel, la conversion est 70% après 30 minutes. Sous pH 10 et 80oC, la conversion est négligeable même après 3 heures.

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47

Alvaro, Vasco Filipe Domingues. "Selective catalytic activity of metals supported on metal(IV) phosphates for heterogeneous reduction." Thesis, University of Liverpool, 1997. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.263780.

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48

Armstrong, Christopher Robert. "Synthesis, spectroscopic, and thermodynamic study of uranyl and neodymium phosphate solid phases." Pullman, Wash. : Washington State University, 2009. http://www.dissertations.wsu.edu/Dissertations/Fall2009/c_armstrong_102809.pdf.

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49

Hunt, Diana Katharine. "Total synthesis of Galbulimima alkaloids. Resin-bound glycosyl phosphates as glycosyl donors." Thesis, Massachusetts Institute of Technology, 2006. http://hdl.handle.net/1721.1/38321.

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Thesis (Ph. D.)--Massachusetts Institute of Technology, Dept. of Chemistry, 2006.
Vita.
Includes bibliographical references.
I. Total Synthesis of Galbulimima Alkaloids. The total synthesis of enantiomerically enriched (+)- and (-)-galbulimima alkaloid 13 is outlined. Sequential use of catalytic cross-coupling and cross-metathesis reactions followed by an intramolecular Diels-Alder reaction provided the required trans-decalin AB ring system and masked the C16-carbonyl as an N-vinyl carbamate for late stage oxidative unveiling as the corresponding C16-enone. Completely diastereoselective introduction of the C-ring via radical cyclization chemistry followed by an enamine-ketone addition for construction of the CDE-ring system allowed rapid entry to the pentacyclic core of these alkaloids. The absolute stereochemistry of natural (-)-galbulimima alkaloid 13 is now unambiguously revised to 2S.
(cont.) II. Resin-bound Glycosyl Phosphates As Glycosyl Donors. Resin-bound glycosyl phosphates were readily accessed on solid support via a three step procedure from support-bound glycals. These resin-bound glycosyl phosphates were successfully used as glycosylating agents for coupling with a series of solution based nucleophiles. The stereochemical outcome of disaccharide formation was dependent on the nature of the linker connecting the saccharide to the polymer. Interestingly, other glycosyl donors such as thioglycosides and trichloroacetimidates did not exhibit this dependence, indicating a different reaction mechanism for glycosylation. III. A Modular Synthesis of FGF-2 Binding Heparin Pentasaccharide. A modular synthesis of FGF-2 binding heparin pentasaccharide is outlined. The synthetic strategy utilizes a disaccharide trichloroacetimidate donor and a uronic acid acceptor as building blocks designed for later application to a fully automated synthesis.
by Diana Katharine Hunt.
Ph.D.

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50

Hatada, Naoyuki. "Low-Temperature Synthesis, Thermodynamic Properties, and Electrical Conduction Properties of Lanthanum Phosphates." 京都大学 (Kyoto University), 2012. http://hdl.handle.net/2433/157583.

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