Wells-Dawson niobium-tungsten mixed polyacid rare earth derivative and preparation method and applications thereof

A technology of derivatives and rare earths, applied in tungsten compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of difficult derivatization and poor stability, and achieve high yield , well-structured, and easy-to-operate effects

Active Publication Date: 2015-05-27
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the authors pointed out that whether in aqueous solution or solid state, Nb 6 P 2 W 12 The stability of these compounds is not good, which brings great difficulties to the further derivatization of such compounds

Method used

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  • Wells-Dawson niobium-tungsten mixed polyacid rare earth derivative and preparation method and applications thereof
  • Wells-Dawson niobium-tungsten mixed polyacid rare earth derivative and preparation method and applications thereof
  • Wells-Dawson niobium-tungsten mixed polyacid rare earth derivative and preparation method and applications thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation method of Wells-Dawson type niobium-tungsten mixed polyacid rare earth derivatives comprises the following steps:

[0027] (1) Synthesize K according to the literature 7 [HNb 6 o 19 ]?13H 2 For O precursors, see Filowitz M, Ho R K C, Klemperer W G, Shum W, Inorg. Chem., 1979, 18, 93–103.

[0028] (2) Synthesize K according to the literature 12 [H 2 P 2 W 12 o 48 ]?24H 2 For O precursors, see Contant R, Inorg. Synth., 1990, 27, 104–111 for literature.

[0029] (3) Under stirring conditions, mix 0.3 g K 7 [HNb 6 o 19 ]?13H 2 O (0.22 mmol), 2 ml of 1 mol / L hydrochloric acid and 0.85 g of K 12 [H 2 P 2 W 12 o 48 ]?24H 2 O (0.21 mmol) was sequentially added to the hydrogen peroxide solution (consisting of 3 ml of 30 wt% hydrogen peroxide and 30 ml of water), stirred at room temperature for 30 minutes and then added with 0.15 g of YCl 3 (0.65 mmol), adjusted the pH to 2.0 with 1 mol / L hydrochloric acid, reacted at 80°C for 8 hours, cooled ...

Embodiment 2

[0031] The preparation method of Wells-Dawson type niobium-tungsten mixed polyacid rare earth derivatives comprises the following steps:

[0032] (1) Synthesize K according to the literature 7 [HNb 6 o 19 ]?13H 2 For O precursors, see Filowitz M, Ho R K C, Klemperer W G, Shum W, Inorg. Chem., 1979, 18, 93–103.

[0033] (2) Synthesize K according to the literature 12 [H 2 P 2 W 12 o 48 ]?24H 2 For O precursors, see Contant R, Inorg. Synth., 1990, 27, 104–111 for literature.

[0034] (3) Under stirring conditions, mix 0.3 g K 7 [HNb 6 o 19 ]?13H 2 O (0.22 mmol), 2 ml of 1 mol / L hydrochloric acid and 0.85 g of K 12 [H 2 P 2 W 12 o 48 ]?24H 2O (0.21 mmol) was added successively to hydrogen peroxide solution (composed of 3 ml 30% hydrogen peroxide and 30 ml water), stirred at room temperature for 40 minutes, and then 0.18 g YCl was added. 3 (0.77 mmol), adjusted the pH to 2.0 with 1 mol / L hydrochloric acid, reacted at 85°C for 8 hours, cooled to room temperatur...

Embodiment 3

[0036] The preparation method of Wells-Dawson type niobium-tungsten mixed polyacid rare earth derivatives comprises the following steps:

[0037] (1) Synthesize K according to the literature 7 [HNb 6 o 19 ]?13H 2 For O precursors, see Filowitz M, Ho R K C, Klemperer W G, Shum W, Inorg. Chem., 1979, 18, 93–103.

[0038] (2) Synthesize K according to the literature 12 [H 2 P 2 W 12 o 48 ]?24H 2 For O precursors, see Contant R, Inorg. Synth., 1990, 27, 104–111 for literature.

[0039] (3) Under stirring conditions, mix 0.38 g K 7 [HNb 6 o 19 ]?13H 2 O (0.28 mmol), 2 ml 1 mol / L hydrochloric acid and 0.85 g K 12 [H 2 P 2 W 12 o 48 ]?24H 2 O (0.21 mmol) was added successively to hydrogen peroxide solution (composed of 3 ml 30% hydrogen peroxide and 30 ml water), stirred at room temperature for 35 minutes, and then 0.27 g YCl was added. 3 (1.16 mmol), adjusted the pH to 2.0 with 1 mol / L hydrochloric acid, reacted at 90°C for 6 hours, cooled to room temperature, f...

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Abstract

The invention discloses a Wells-Dawson niobium-tungsten mixed polyacid rare earth derivative. The chemical formula of the derivative is K8 [H14{Nb12P4W24O122}2{Y(H2O)4.5}4{Nb4O4(OH)6}].18H2O, a crystal of the derivative belongs to an orthorhombic system, a space group is Fddd, and cell parameters are as follows: a = 24.075(4) angstrom, b = 43.886(8) angstrom, and c = 70.192(11) angstrom. The derivative is prepared from potassium hexaniobate, hexavacant Wells-Dawson phosphowolframate and rare earth ions through reacting under conventional aqueous solution conditions. The derivative is high in stability, and has a photocatalytic hydrogen production performance; and in addition, the preparation process is simple, easy to operate, low in cost and high in yield, therefore, the derivative has a potential application prospect.

Description

technical field [0001] The invention belongs to the technical field of new polyacid chemical materials, and in particular relates to a Wells-Dawson type niobium-tungsten mixed polyacid rare earth derivative, a preparation method and application of the derivative. Background technique [0002] Polyacids are usually composed of early transition metal ions (such as Mo 6+ , W 6+ , V 5+ , Nb 5+ , Ta 5+ ) is a class of polynuclear complexes formed by connecting oxygen atoms, and plays an increasingly important role in catalysis, materials, magnetism, medicine, nanoscience and other fields (see Müller A, Peters F, Pope M T, Gatteschi D, Chem. Rev. , 1998, 98, 239?271; Long D-L, Burkholder E, Cronin L, Chem. Soc. Rev., 2007, 36, 105-121; Long D-L, Tsunashima R, Cronin L, Angew. Chem. Int. Ed. , 2010, 49, 1736–1758; Li Feng-Yan, Xu Lin, Dalton Trans. , 2011, 40, 4024–4034; Du Dong-Ying, Yan Li-Kai, Su Zhong-Min, Li Shun-Li, Lan Ya-Qian, Wang En-Bo, Coord. Chem. Rev. , ...

Claims

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Application Information

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IPC IPC(8): C01G41/00B01J31/18
CPCB01J27/195C01B25/45C01P2002/82
Inventor 张东娣马鹏涛王敬平牛景杨
Owner HENAN UNIVERSITY
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