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Immobilized tungstophosphoric heteropoly acid catalyst and use thereof

A technology of phosphotungstic heteropolyacid and catalyst, which is applied in the direction of physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, chemical industry, etc., can solve the problem of high catalyst use cost, reduce production cost, Long life and easy recycling

Active Publication Date: 2016-06-01
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of a catalyst that can be used to catalyze the epoxidation of cis-acrylphosphonic acid to synthesize left phosphorus and right ammonium salt, so as to overcome the defect that the cost of catalyst is too high in the production process of fosfomycin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Catalyst preparation:

[0013] Weigh 3.32g of sodium tungstate into 10mL of deionized water, stir to dissolve it completely, add 3.94g of 6mol / L HCl, a precipitate is formed, stir to fully react. Add 7.94g 30% H 2 o 2 Aqueous solution, the precipitate dissolves rapidly, and after heating to 60°C for 30 minutes, it becomes a pale yellow solution. Accurately add 1 mL of 85% H 3 PO 4 Solution, continue to stir and react for 10 minutes to obtain peroxyphosphotungstic acid solution. Accurately weigh 2.55g of tetrabutylammonium bisulfate and dissolve it in 10mL of deionized water, then slowly add it dropwise into the above solution of phosphotungstic acid peroxygen under stirring, continue to stir for 10min after dropping, filter with suction, and dry the filter cake at room temperature to obtain White solid, namely {PO 4 [WO(O 2 ) 2 ] 4}((n-Bu) 4 N) 3 .

[0014] Weigh 0.87g of the above solid and dissolve it in 5mL of dichloromethane and 1.5mL of 30% H 2 o 2 aq...

Embodiment 2

[0020] Catalyst preparation:

[0021] Weigh 3.32g of sodium tungstate into 10mL of deionized water, stir to dissolve it completely, add 1.97g of 12mol / L HCl, a precipitate is formed, stir to make it fully react. Add 7.94g 30% H 2 o 2 Aqueous solution, the precipitate dissolves rapidly, and after heating to 50°C for 30 minutes, it becomes a pale yellow solution. Accurately add 1 mL of 85% H 3 PO 4 Solution, continue to stir and react for 10 minutes to obtain peroxyphosphotungstic acid solution. Accurately weigh 1.71g of tetrabutylammonium chloride and dissolve it in 10mL of deionized water, then slowly add it dropwise into the above-mentioned peroxyphosphotungstic acid solution under stirring, continue to stir for 10min after dropping, filter with suction, and dry the filter cake at room temperature to obtain White solid, namely {PO 4 [WO(O 2 ) 2 ] 4}((n-Bu) 4 N) 3 .

[0022] Weigh 1.17 g of the above solid and dissolve it in 10 mL of chloroform and 2 mL of 30% H 2...

Embodiment 3

[0028] Catalyst preparation:

[0029] Weigh 3.32g of sodium tungstate in 10mL of deionized water, stir to dissolve it completely, add 0.99g of 6mol / L H 2 SO 4 , a precipitate is formed, stir to make it fully react. Add 7.94g 30% H 2 o 2 Aqueous solution, the precipitate dissolves rapidly, and after heating to 50°C for 30 minutes, it becomes a pale yellow solution. Accurately add 1 mL of 85% H 3 PO 4Solution, continue to stir and react for 10 minutes to obtain peroxyphosphotungstic acid solution. Accurately weigh 2.42g of tetrabutylammonium bromide and dissolve it in 10mL of deionized water, then slowly add it dropwise into the above-mentioned peroxyphosphotungstic acid solution under stirring, continue to stir for 10min after dropping, filter with suction, and dry the filter cake at room temperature to obtain White solid, namely {PO 4 [WO(O 2 ) 2 ] 4}((n-Bu) 4 N) 3 .

[0030] Weigh 0.76g of the above solid and dissolve it in 5mL of dichloromethane and 1.5mL of 30...

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Abstract

The invention relates to a synthesis method of an immobilized tungstophosphoric heteropoly acid catalyst and a use of the immobilized tungstophosphoric heteropoly acid catalyst in cis-propenylphosphonic acid epoxidation. The synthesis method of the immobilized tungstophosphoric heteropoly acid catalyst comprises 1, synthesizing low-carbon chain phosphotungstic heteropoly acid quaternary ammonium salt and 2, loading the phosphotungstic heteropoly acid quaternary ammonium salt on resin to obtain the immobilized tungstophosphoric heteropoly acid catalyst. The catalyst is prepared from easily available raw materials, effectively catalyzes cis-propenylphosphonic acid epoxidation to synthesize fosfomycin phenylethylamine salt, is convenient for recovery, has a long service life and can be recycled 5 times. The catalyst can reduce a fosfomycin phenylethylamine salt production cost and satisfies the current green chemical and atom economic requirements.

Description

technical field [0001] The invention relates to the synthesis of a solid-supported phosphotungstic heteropolyacid catalyst and its application in the epoxidation reaction of cis-acrylphosphonic acid. Synthesis of solid-supported catalyst with polystyrene resin as the carrier and its catalyzed epoxidation of cis-acrylphosphonic acid to synthesize left phosphorus and right amine salt. Background technique [0002] Fosfomycin is a broad-spectrum antibacterial drug with low toxicity and side effects. It can inhibit the synthesis of bacterial cell walls. It is a fungicide during the breeding period and has a wide range of applications. In the production process of fosfomycin, the epoxidation reaction of cis-acrylophosphate is one of the key steps in the synthesis of fosfomycin. At present, sodium tungstate is used as the epoxidation catalyst in industry. The catalyst has high activity and can realize epoxidation of cis-acrylphosphonic acid at a relatively low temperature, but th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18C07F9/655
CPCY02P20/50Y02P20/584
Inventor 史海赵许群王晓东张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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