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Citation: LIU Hong-Xia, YANG Chun, ZHOU Jia-Hong. Synthesis of Ti(Ⅳ)-Substituted Keggin-type Polyoxometalates with Titanium Isopropoxide as Ti Source[J]. Chinese Journal of Applied Chemistry, ;2007, 24(9): 1000-1004. shu

Synthesis of Ti(Ⅳ)-Substituted Keggin-type Polyoxometalates with Titanium Isopropoxide as Ti Source

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a College of Chemistry and Environment Science, Nanjing Normal University, Nanjing 210097;
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b Analysis and Testing Center of Nanjing Normal University, Nanjing

Corresponding author: YANG Chun,
Received Date: 6 October 2006
Available Online: 8 January 2007
Fund Project: 国家自然科学基金资助项目(20473037) (20473037)江苏省教育厅自然科学基金资助项目(04KJB150069) (04KJB150069)国家人事部留学人员科技活动项目(2005103SB9BH51) (2005103SB9BH51)

The Ti(Ⅳ)-substituted tungstophosphate and tungstosilicate polyoxometalates(Bu₄N⁺ salt or Me₄N⁺ salt) were synthesized under the acid condition(pH=2) with Ti(O-iPr)₄ as Ti source. The structures and cation contents of the samples were characterized by IR, ³¹P NMR, ¹H NMR and TG-DTA. The states of the samples, i.e., dimer(anhydride form), monomer, protonated monomer, as well as the interconversion between the states were also investigated. The IR spectra of the samples show that both the tungstophosphate and tungstosilicate contain Ti-O-Ti linkages, indicating that the compounds are Ti(Ⅳ)-substituted polyoxometalate dimers or contain dimers. This has also been confirmed by the contents of Me₄N⁺ measured by TG-DTA experiments. ³¹P NMR and ¹H NMR further reveal that Ti(Ⅳ)-substituted tungstophosphate sample is a mixture of protonated monomer and dimer. It has also been found that acidic medium is necessary for the formation of protonated monomer and dimer. The stability of the dimer of the tungstophosphate is lower; a pure monomer can be obtained by treating the mixture with a base (Bu₄NOH). However, the dimer of tungstosilicate is stable under the same condition.
- polyoxometalates,
- Keggin structure,
- Ti(Ⅳ)-substitution,
- titanium isopropoxide
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