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Supported polyoxometallate crystalline catalyst and preparation method thereof

A polyoxometalate and catalyst technology, applied in the field of chemical materials, can solve the problems of difficulty in catalyst separation and recovery, limit the catalytic performance of solid catalysts, and small specific surface area, and achieve obvious industrial application prospects, low cost, and simple preparation methods Effect

Inactive Publication Date: 2010-10-27
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the homogeneous catalytic reaction of polymetallic hydrochloride has the advantages of high activity, good selectivity and mild conditions, there are also problems such as difficulty in catalyst separation and recovery.
On the other hand, the specific surface area of ​​solid polyoxometalates is usually very small (2 g -1 ), limiting its catalytic performance as a solid catalyst

Method used

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  • Supported polyoxometallate crystalline catalyst and preparation method thereof
  • Supported polyoxometallate crystalline catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: H 3 [(Cu 4 Cl) 3 (BTC) 8 ] 2 [PW 12 o 40 ]·(C 4 h 12 N) 6 ·3H 2 Preparation of O crystalline catalyst

[0017] Na was prepared according to the literature method 3 PW 12 o 40 ·xH 2 O (Rocchiccioli-Deltcheff et al. Inorg. Chem. 1983, 22, 207-216). CuCl 2 2H 2 O, Na 3 PW 12 o 40 ·xH 2 O. Trimellitic acid and tetramethylammonium hydroxide were mixed in water at a material ratio of 9:1:10:20, and the stirring was continued at room temperature. The final pH value of the mixture was 4. The mixture was charged into a Teflon-lined autoclave and heated at 180°C for 50 hours to obtain olive green cubic crystals. After fully washing with deionization, it was collected by filtration to obtain pure compound H 3 [(Cu 4 Cl) 3 (BTC) 8 ] 2 [PW 12 o 40 ]·(C 4 h 12 N) 6 ·3H 2 O, the crystal structure belongs to the cubic crystal system, the space group Fm-3m, and the unit cell parameters are as follows: α=β=γ=90°,

Embodiment 2

[0018] Example 2: H 3 [(Cu 4 Cl) 3 (BTC) 8 ] 2 [PMo 12 o 40 ]·(C 4 h 12 N) 6 Preparation of Crystalline Catalysts

[0019] Na was prepared according to the literature method 2 HPMo 12 o 40 14H 2 O (Rocchiccioli-Deltcheff et al. Inorg. Chem. 1983, 22, 207-216). CuCl 2 2H 2 O, Na 2 HPMo 12 o 40 14H 2 O. Trimellitic acid and tetramethylammonium hydroxide were mixed in water according to the mass ratio of 10:1:8:16, and the stirring was continued at room temperature, and the final pH value of the mixture was 4.5. The mixture was charged into a Teflon-lined autoclave and heated at 180 °C for 72 hours to obtain green cubic crystals. After fully washing with deionization, it was collected by filtration to obtain pure compound H 3 [(Cu 4 Cl) 3 (BTC) 8 ] 2 [PMo 12 o 40 ]·(C 4 h 12 N) 6 , the crystal structure belongs to the cubic crystal system, the space group Fm-3m, and the unit cell parameters are as follows: α=β=γ=90°,

Embodiment 3

[0020] Example 3: H 3 [(Cu 4 Cl) 3 (BTC) 8 ] 2 [AsW 12 o 40 ]·(C 4 h 12 N) 6 ·3H 2 Preparation of O crystalline catalyst

[0021] Na was prepared according to the literature method 3 AsW 12 o 40 ·xH 2 O (Rocchiccioli-Deltcheff et al. Inorg. Chem. 1983, 22, 207-216). CuCl2 2H 2 O, Na 3 AsW 12 o 40 ·xH 2 O. Trimellitic acid and tetramethylammonium hydroxide were mixed in water according to the mass ratio of 8:1:10:20, and the stirring was continued at room temperature, and the final pH value of the mixture was 5. The mixture was charged into a Teflon-lined autoclave and heated at 195 °C for 50 hours to obtain blue cubic crystals. After fully washing with deionization, it was collected by filtration to obtain pure compound H 3 [(Cu 4 Cl) 3 (BTC) 8 ] 2 [AsW 12 o 40 ]·(C 4 h 12 N) 6 ·3H 2 O, the crystal structure belongs to the cubic crystal system, the space group Fm-3m, and the unit cell parameters are as follows: α=β=γ=90°,

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Abstract

The invention belongs to the technical field of chemical materials, and relates to a supported polyoxometallate crystalline catalyst and a preparation method thereof. The crystalline material is formed by using a three-dimensional porous metal-organic frame as a main body with a supported Keggin type polyoxometallate in the pore canal and is prepared by reaction of polyoxometallate with trimesic acid, copper salt and ammonium salt under the condition of hydrothermal self-generated pressure. The component formula is as follows: Hx[(Cu4Cl)3(BTC)8]2[POM].(C4H12N)6.yH2O, wherein BTC is trimesic acid, and POM is Keggin type polyoxometallate. The material has greater specific surface area and can realize that the catalyst and a reactant are contacted in molecular size. At the same time, the material has high stability, simple preparation method, low cost and is easy to recycle.

Description

technical field [0001] The invention belongs to the technical field of chemical materials, and relates to a class of crystalline catalysts loaded with polyoxometalates based on porous metal-organic frameworks and a preparation method thereof. Background technique [0002] Polyoxometalates, as new and efficient catalysts, are currently the most important application. They act as excellent catalysts in both homogeneous and heterogeneous systems. Although the homogeneous catalytic reaction of polymetallic hydrochloride has the advantages of high activity, good selectivity and mild conditions, there are also problems such as difficulty in catalyst separation and recovery. On the other hand, the specific surface area of ​​solid polyoxometalates is usually very small (<10m 2 g -1 ), limiting its catalytic performance as a solid catalyst. Therefore, the combination of polyoxometalates and porous supports forms a new hybrid material based on polyoxometalates, and as a support...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/34
Inventor 刘术侠马凤吉
Owner NORTHEAST NORMAL UNIVERSITY
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