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Solvothermal Synthesis and Characterization of Novel Titanium Phosphate and Manganese Phosphate
Author: HouZhiYang
Tutor: GuoYangHong
School: Jilin University
Course: Inorganic Chemistry
Keywords: Solvothermal Chirality Magnetic properties
CLC: O611.3
Type: Master's thesis
Year: 2006
Downloads: 79
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Abstract
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Inorganic microporous materials have popular application incatalysis, adsorption, ion-exchange, separation and host-guestassemblies due to their unique pore architectures. And the rationaldesign and synthesis of new microporous compounds, as well as thedevelopment of new synthetic ways are becoming the topics ofmicroporous chemistry. In the last decade, the synthesis of newmaterials that might combine the nanoporosity of zeolites with themagnetic and optical properties, electronic conductivity and ferrodlectricity of transition metal phosphates such as TiPOs, VPOs, FePOs,ZnPOs and CoPOs have been reported in the literature.Many of thesematerials exhibit unique structures and may have potential applicationsin catalysis and magnetic field. The successful syntheses of these newcompounds with open-framework open a new field for themicroporous compounds.Chiral molecular sieves attract considerable attention, because oftheir extensive application in enantioselective catalysis, separation andpharmacy. The goal of this work is to synthesis and preparation ofchiral titanium phosphates and manganese phosphate continuously andsystematically by solvothermal routes. And also to explore thesynthesis of coordination polymers by hydrothermal.A novel titanium phosphate [TiO(HPO4)2·(NH3C3H6NH3)] hasbeen synthesized by solvothermal synthesis. The crystallographic dataof the compound is a= 7.1882(14)?, b=8.6324(17)?, c=19.386(4)?,V= 1202.9(4) ?3,space group: Orthorhombic, P21221,Z=4.Theone-dimensional chiral chain is built from the strictly alternating TiO6pyramidal and HPO4 tetrahedron that are lined through their vertices.The chains are connect by H bond .Using solvothermal synthesis method, transitional metalmanganese atom which have special reaction activity, alterable bondvalue and various structural group as framework element, wesynthesize one new composition and structure of 2D layeropenframework manganese phosphate[Mn2(PO4)(H2PO4)(CH2NHCH2)]. The crystallographic data of thecompound is a=6.5878(9)?, b=22.219(3)?, c=9.3213(12)?, V=1364.2(3) ?3,space group: Orthorhombic, Pnma,Z=4. The compoundhas the same character-the bond values of manganese atoms offramework are quadrivalence. The 2 D layer framework structure of[ Mn2(PO4)(H2PO4) (CH2NHCH2) ] is built from the strictlyalternating MnO6 pyramidal and MnO5 triangular bipyramidalgeometry and PO4 tetrahedron. The Triethylenetetramine counter ionsinteract with the inorganic layers through O (inorganic layer)-H-N(counter ion) hydrogen bonds. All the N-H bonds of the counter ionsinvolved in the hydrogen bonds with the terminal oxygen atoms form akind of 2D structure.Using hydrothermal synthesis method, propanediamine astemplate, we first prepared the novel titanium oxalate[Ti4O4(C2O4)8·4(C3N2H12) ·2H2O] . The compound is a = 14.2192(18)?, b = 14.2192(18) ?, c = 12.546(2) ?, Z =4 V=2536.6(6) ?3, spacegroup : tetragonal. The compound is composed of Ti4O4(C2O4)88-polyoxometalates anions and propanediamine cations. The anionsmake up of four Ti atoms from O atoms-shared. Noveal frameworkelements and connction manners showed that it is possible tosynthesize the new compound of non-phosphate open framework.
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