Hydrothermal Synthesis and Structural\nCharacterization of Three Organically Templated\nTitanium Phosphates:  Ti&lt;sub&gt;2&lt;/sub&gt;(HPO&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;(PO&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;·C&lt;sub&gt;2&lt;/sub&gt;N&lt;sub&gt;2&lt;/sub&gt;H&lt;sub&gt;10&lt;/sub&gt;,\nTi&lt;sub&gt;3&lt;/sub&gt;(H&lt;sub&gt;2&lt;/sub&gt;PO&lt;sub&gt;4&lt;/sub&gt;)(HPO&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;3.5&lt;/sub&gt;(PO&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;·C&lt;sub&gt;2&lt;/sub&gt;N&lt;sub&gt;2&lt;/sub&gt;H&lt;sub&gt;10&lt;/sub&gt;, and\nTi&lt;sub&gt;7&lt;/sub&gt;(HPO&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;6&lt;/sub&gt;(PO&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;6&lt;/sub&gt;·C&lt;sub&gt;3&lt;/sub&gt;N&lt;sub&gt;2&lt;/sub&gt;H&lt;sub&gt;12&lt;/sub&gt;

Yunling Liu (1420054); Zhan Shi (704217); Yunlong Fu (1536427); Wei Chen (23863); Baozong Li (1621120); Jia Hua (410225); Wuyang Liu (2953659); Feng Deng (553812); Wenqin Pang (2537944)

JOURNAL ARTICLE

Hydrothermal Synthesis and Structural\nCharacterization of Three Organically Templated\nTitanium Phosphates: Ti2(HPO4)2(PO4)2·C2N2H10,\nTi3(H2PO4)(HPO4)3.5(PO4)2·C2N2H10, and\nTi7(HPO4)6(PO4)6·C3N2H12

Yunling Liu (1420054)Zhan Shi (704217)Yunlong Fu (1536427)Wei Chen (23863)Baozong Li (1621120)Jia Hua (410225)Wuyang Liu (2953659)Feng Deng (553812)Wenqin Pang (2537944)

Year: 2016 Journal: OPAL (Open@LaTrobe) (La Trobe University) Publisher: La Trobe University

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Abstract

Three organically templated titanium phosphates with the formulas Ti2(HPO4)2(PO4)2·C2N2H10 (1), Ti3(H2PO4)(HPO4)3.5(PO4)2·C2N2H10 (2), and Ti7(HPO4)6(PO4)6·C3N2H12 (3) have\nbeen prepared hydrothermally from titanium powder, phosphoric acid, and structure-directing organic amines. The as-synthesized products are characterized by powder X-ray\ndiffraction, 31P MAS NMR spectroscopy, IR spectroscopy, and thermogravimetric and\ndifferential thermal analyses (TG-DTA). The structures have been solved by single-crystal\nX-ray diffraction analysis. Crystal data for 1: triclinic, P1̄, a = 6.3066(17) Å, b = 10.181(4)\nÅ, c = 12.644(3) Å, α = 102.14(2)°, β = 102.49(3)°, γ = 90.00(2)°, Z = 2. Crystal data for 2: \ntriclinic, P1̄, a = 10.3183(9) Å, b = 10.7501(10) Å, c = 10.8315(10) Å, α = 73.436(2)°, β =\n79.648(2)°, γ = 83.260(2)°, Z = 2. Crystal data for 3: trigonal, R3̄, a = 16.4993(15) Å, b =\n16.4993(15) Å, c = 12.704(3) Å, Z = 3. Their frameworks are all built up with TiO6 octahedra\nand PO4, PO2(OH)2, PO3(OH), and/or PO2(O)(OH) tetrahedral units. Compound 1 is an\nethylenediamine intercalated layered titanium phosphate in which the layers are similar\nto that of γ-type titanium phosphate. Both 2 and 3 are of open-framework type, and the\ndiprontonated organic amine molecules are entrapped in 12-membered-ring channels for 2\nand 8-membered-ring channels for 3.

Keywords:

Hydrothermal synthesis Thermogravimetric analysis Titanium Crystal structure Phosphoric acid Amine gas treating Molecule Hydrothermal circulation Infrared spectroscopy

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