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Method for preparing fluorinated chain-containing palladium catalyst and application thereof

The technology of a palladium catalyst and carbon chain is applied in the preparation of a fluorine-containing carbon chain palladium catalyst and the application field in the synthesis of vinyl carboxylates, which can solve the problems of affecting catalyst recovery, easy leakage of the catalyst, low catalytic activity, etc. Low, mild conditions, good catalytic activity

Inactive Publication Date: 2017-01-04
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above-mentioned technologies generally use palladium salt catalyst, but the disadvantage is that the catalyst is easy to leak, which affects the recovery of the catalyst
Using Pd / C as a catalyst can overcome the above difficulties, and the catalyst is easy to recycle, but its catalytic activity is much lower than that of palladium salt catalysts.

Method used

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  • Method for preparing fluorinated chain-containing palladium catalyst and application thereof
  • Method for preparing fluorinated chain-containing palladium catalyst and application thereof
  • Method for preparing fluorinated chain-containing palladium catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1. Palladium perfluorohexanoate (Pd(OCOC 5 f 11 ) 2 ) preparation

[0025] Under a nitrogen atmosphere, add 100 mg (0.446 mmol) of palladium acetate and 420 mg (1.33 mmol) of perfluorohexanoic acid into the flask, stir and react at 60°C for 24 hours, cool to room temperature, and remove excess perfluorohexanoic acid by filtration to obtain a gray solid , washed with petroleum ether, and dried to obtain 150 mg of product, with a yield of 46%.

Embodiment 2

[0026] Embodiment 2. Palladium perfluorohexanoate (Pd(OCOC 5 f 11 ) 2 ) preparation

[0027] Under a nitrogen atmosphere, add 100 mg (0.446 mmol) of palladium acetate and 420 mg (1.33 mmol) of perfluorohexanoic acid into the flask, add 5 mL of NMP, stir and react at 60 °C for 24 h, cool to room temperature, and remove volatiles to obtain a gray solid. Washed with petroleum ether and dried to obtain 200 mg of product with a yield of 61%.

Embodiment 3

[0028] Embodiment 3. Palladium perfluorohexanoate (Pd(OCOC 5 f 11 ) 2 ) preparation

[0029] Under a nitrogen atmosphere, add 100 mg (0.43 mmol) of palladium nitrate and 420 mg (1.33 mmol) of perfluorohexanoic acid into the flask, stir and react at 80°C for 12 hours, cool to room temperature, and remove excess perfluorohexanoic acid by filtration to obtain gray The solid was washed with petroleum ether and dried to obtain 180 mg of the product, with a yield of 57%.

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PUM

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Abstract

The invention discloses a method for preparing a fluorinated chain-containing palladium catalyst. A palladium-containing precursor and perfluorocarboxylic acid react according to a molar ratio of 1:2-3, the reaction temperature is 60-100 DEG C, the reaction time is 2-24 h, and after the reaction is over, the fluorinated chain-containing palladium catalyst product is obtained through cooling, filtration, washing and drying. The invention further discloses application of the catalyst to preparation of carboxylic acid vinyl ester. The catalyst is used for preparing the carboxylic acid vinyl ester and has the advantages that the carboxylic acid vinyl ester is simple in process and high in yield, a catalytic system is easy to separate, and the carboxylic acid vinyl ester is low in cost, safe and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a preparation method of a fluorine-containing carbon chain palladium catalyst and its application in synthesizing vinyl carboxylate. Background technique [0002] Traditionally, acrylate compounds have been widely used as polymer monomers in polymer materials. However, acrylic compounds are often highly irritating, highly volatile, and carcinogenic, and some countries have restricted their use. Vinyl carboxylate is a new polymer monomer and a substitute for acrylate. Vinyl benzoate is an important vinyl carboxylate. Vinyl benzoate is a basic chemical raw material for synthesizing modified polymer materials. It is widely used in paints, adhesives, coating preparations, and cement slurry mixtures. Finding an economical and convenient synthesis method of vinyl carboxylate has always been one of the goals of chemical research. [0003] At present, the synthesis of vinyl benzoate...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C53/21C07C67/10C07C69/78B01J31/04B01J31/22
CPCC07C51/412B01J31/04B01J31/183B01J2231/49B01J2531/0241B01J2531/824C07C67/10C07C53/21C07C69/78
Inventor 王志光陈贵夫姜赟周建华余红明李宏峰
Owner JUHUA GROUP TECH CENT