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Preparation method of vinyl carboxylate

A technology of vinyl carboxylate and vinyl acetate, which is applied in the field of fine chemical new catalysts, can solve the problems of high price, high cost, and pollution, and achieve the advantages of simple preparation method, low equipment corrosion, and improved dispersion Effect

Active Publication Date: 2012-08-08
JIANGSU YIDA CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, tin catalysts are more difficult to separate and remove completely after the reaction, thus easily causing the reaction product to become darker in color. Therefore, they cannot be used in those occasions that require higher catalyst residues; and organotin catalysts are expensive. It has practical application value in industry, and the problem of repeated reuse of catalyst must be solved
[0009] In the above methods, the catalysts are used directly, which is not only costly, but also difficult to post-process, which will cause pollution. Therefore, it is urgent to develop new catalysts that are non-corrosive, non-polluting, and easy to separate.

Method used

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  • Preparation method of vinyl carboxylate

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0030] Weigh HgSO 4 1 g of powder was dissolved in 0.1 mol / L HCl and placed in a flask, and 5 g of treated activated carbon was added (the activated carbon was pretreated with 30% nitric acid solution), stirred and impregnated at 60 °C for 10 h, evaporated The solvent was removed, dried at 100 °C to constant weight, and calcined at 200 °C for 2 h to obtain supported HgSO 4 / C solid catalyst.

[0031] Add 23.7 g (0.15 mol) of nonanoic acid, 90.3 g (1.05 mol) of vinyl acetate, and 3.42 g (3.0 %) of catalyst into a 500 mL four-neck flask equipped with a thermometer, a condenser tube and a stirrer, accounting for the total mass of the reactants. Mass percent, the same below), heated to reflux, stirred for 10 h, cooled to room temperature, filtered to separate the catalyst, and gas chromatography analyzed the contents of each component of the reaction product as follows:

[0032] components content(%) vinyl acetate 69.6 nonanoic acid 3.1 acetic acid 6...

example 2

[0035] Weigh HgSO 4 1 g of powder, dissolved in 0.1 mol / L HCl, was placed in a flask, 5 g of activated carbon treated with 30% nitric acid solution was added, stirred and impregnated at 60 °C for 10 h, evaporated to remove the solvent, and dried at 100 °C to Constant weight, calcined at 200 °C for 2 h to obtain supported HgSO 4 / C solid catalyst.

[0036] Add 17.4 g (0.15 mol) of hexanoic acid, 90.3 g (1.05 mol) of vinyl acetate, and 3.23 g (3.0%) of catalyst into a 500 mL four-necked flask equipped with a thermometer, condenser and stirrer, and heat up to reflux. Stir the reaction for 10 h, cool to room temperature, filter and separate the catalyst, and analyze the contents of each component of the reaction product by gas chromatography as follows:

[0037] components content(%) vinyl acetate 73.3 caproic acid 1.9 acetic acid 7.4 product 17.4

[0038] The calculated yield of vinyl hexanoate was 87.9%.

example 3

[0040] Weigh HgSO 4 1 g of powder, dissolved in 0.1 mol / L HCl, was placed in a flask, 5 g of activated carbon treated with 30% nitric acid solution was added, stirred and impregnated at 60 °C for 10 h, evaporated to remove the solvent, and dried at 100 °C to Constant weight, calcined at 200 °C for 2 h to obtain supported HgSO 4 / C solid catalyst.

[0041] Add 13.2 g (0.15 mol) of butyric acid, 90.3 g (1.05 mol) of vinyl acetate, and 3.11 g (3.0%) of catalyst into a 500 mL four-necked flask equipped with a thermometer, condenser and stirrer, and heat up to reflux. Stir the reaction for 10 h, cool to room temperature, filter and separate the catalyst, and analyze the contents of each component of the reaction product by gas chromatography as follows:

[0042] components content(%) vinyl acetate 76.2 butyric acid 1.5 acetic acid 7.7 product 14.6

[0043] The calculated vinyl butyrate yield was 88.5%.

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Abstract

The invention relates to a preparation method of a vinyl carboxylate. According to the method, a carboxylic acid and vinyl acetate are subjected to a vinyl group exchange reaction under refluxing in the presence of a supported HgSO4 / C solid catalyst to obtain a reaction solution containing a corresponding vinyl carboxylate. The method which allows the catalyst to be simply prepared, have a high catalytic activity and be easily separated from products is a high-efficiency environmental-protection production method.

Description

technical field [0001] The invention relates to a preparation method of vinyl carboxylate, which belongs to the technical field of new catalysts for fine chemicals. Background technique [0002] Vinyl carboxylate is an important organic intermediate, because the structure contains active functional groups - double bonds, which can undergo addition and polymerization reactions, and its homopolymers or copolymers are used in adhesives, coatings, antirust agents, etc. Both have applications, unsaturated vinyl carboxylate, can also be used as cross-linking agent, photosensitive resin material. Polymer of high-grade saturated carboxylic acid vinyl ester (carboxylic acid with 8-18 carbon atoms), the more carboxylic acid carbon atoms, the softer it is, the colorless rubber-like color with 8-12 carbon atoms, and more than 12 carbon atoms It is waxy. Mainly used as a comonomer, copolymerized with vinyl chloride, vinyl acetate or acrylonitrile, acrylic acid and its esters, or styren...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/24C07C69/78C07C67/10B01J27/053
Inventor 刘准朱新宝王利娟吴建磊张虎曹惠庆
Owner JIANGSU YIDA CHEM
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