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Preparation method of fluorine-containing hydroxyphenyl organic acid alkenyl ester demoulding intermediate

A technology of fluorine-containing hydroxyphenyl and organic acids, which is applied in the field of mold release additive synthesis, can solve the problems of high-efficiency fluorine mold release agents relying on imports, and achieve improved mold release efficiency and product processing quality, good economic and social benefits, The effect of simple and easy reaction operation

Inactive Publication Date: 2017-06-27
修建东
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some foreign companies and research institutions have done a lot of research on fluorine release agents, but there are few domestic reports on this research and development. The existing high-efficiency fluorine release agents basically rely on imports.

Method used

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  • Preparation method of fluorine-containing hydroxyphenyl organic acid alkenyl ester demoulding intermediate
  • Preparation method of fluorine-containing hydroxyphenyl organic acid alkenyl ester demoulding intermediate
  • Preparation method of fluorine-containing hydroxyphenyl organic acid alkenyl ester demoulding intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a four-neck flask equipped with a stirring device, a reflux condenser and a thermometer, add 100 mL of N,N-dimethylacetamide, 25 g of p-phenol acetic acid and 1.2 g of decarboxylated hexafluoropropylene oxide dimer, turn on the stirring, Slowly add 25 grams of triethylamine, keep the temperature of 25℃~35℃ in the water bath, carry out the nucleophilic substitution reaction for 6 hours, add 60mL of water to the four-neck flask to dilute the reaction material, and add the mass concentration of 20 under stirring. % Sodium hydroxide solution, adjust the pH value to about 10, filter, take the filtrate, slowly pour a dilute hydrochloric acid solution with a mass concentration of 20% into the filtrate under stirring, adjust the pH value to about 1.0, precipitate solid products, filter Then the filter cake was washed repeatedly with water and dried to obtain the hydroxyphenyl organic acid substituted by the decarboxylated hexafluoropropylene oxide dimer, and the hydroxyphenyl ...

Embodiment 2

[0025] In a four-neck flask equipped with a stirring device, a reflux condenser and a thermometer, add 100 mL of N,N-dimethylacetamide, 30 grams of p-phenol propionic acid and 60 grams of decarboxylated hexafluoropropylene oxide dimer, and turn on the stirring , Slowly add 1.8 g of triethylamine, keep the temperature of 25℃~35℃ in the water bath, carry out the nucleophilic substitution reaction for 7 hours, add 60mL of water to the four-neck flask to dilute the reaction material, add the mass concentration of 20% sodium hydroxide solution, adjust the pH value to about 10, filter, take the filtrate, slowly pour a dilute hydrochloric acid solution with a mass concentration of 20% into the filtrate under stirring, adjust the pH value to about 1.0, and precipitate a solid product. After filtration, the filter cake was washed repeatedly with water and dried to obtain decarboxylated hexafluoropropylene oxide dimer substituted hydroxyphenyl organic acid, and decarboxylated hexafluoropr...

Embodiment 3

[0027] In a four-neck flask equipped with a stirring device, a reflux condenser and a thermometer, add 100 mL of N,N-dimethylacetamide, 20 grams of m-phenolic acid and 50 grams of decarboxylated hexafluoropropylene oxide dimer, turn on the stirring, Slowly add 1.0 g of triethylamine, keep the temperature of 25℃~35℃ in the water bath, carry out the nucleophilic substitution reaction for 5 hours, add 60mL water to the four-neck flask to dilute the reaction material, and add the mass concentration of 20 under stirring. % Sodium hydroxide solution, adjust the pH value to about 10, filter, take the filtrate, slowly pour a dilute hydrochloric acid solution with a mass concentration of 20% into the filtrate under stirring, adjust the pH value to about 1.0, precipitate solid products, filter Then the filter cake was washed repeatedly with water and dried to obtain the hydroxyphenyl organic acid substituted by the decarboxylated hexafluoropropylene oxide dimer, and the hydroxyphenyl orga...

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Abstract

The invention discloses a method for preparing a release intermediate of fluorine-containing hydroxyphenyl organic acid alkenyl ester, which is characterized in that: hydroxyphenyl organic acid and decarboxylated hexafluoropropylene oxide dimer undergo nucleophilic substitution reaction, The obtained sodium hydroxyphenyl organic acid substituted by hexafluoropropylene oxide dimer is acidified with acid solution to obtain the hydroxyphenyl organic acid substituted by decarboxylated hexafluoropropylene oxide dimer. And under the polymerization inhibitor, the hydroxyphenyl organic acid substituted by the decarboxylated hexafluoropropylene oxide dimer is finally esterified with propenyl alcohol to obtain the fluorine-containing hydroxyphenyl organic acid alkenyl ester release intermediate; the Fluorine-based release intermediates can be further reacted with acrylic compounds to synthesize high-efficiency fluorine-containing release agents, which can improve release efficiency and product processing quality, meet the high-end needs of the market, and have good economic and social benefits.

Description

Technical field [0001] The invention relates to the technical field of the synthesis of mold release additives, in particular to a method for preparing a mold release intermediate of fluorine-containing hydroxyphenyl organic acid alkenyl ester. Background technique [0002] The release agent is a functional substance between the mold and the organic polymer material or other products. It prevents the molded products, laminated products, spinning parts, etc. of rubber, plastic, polyurethane and other elastomer materials and other materials. The substance is bonded to the surface of the mold or metal plate, and it is a kind of processing aid that is easy to detach. Excellent release agent has greater tensile strength. The release agent has chemical resistance, heat resistance and stress properties, and is not easy to decompose or wear; the release agent adheres to the mold and does not transfer to the processed part , Does not interfere with painting or other secondary processing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/84
CPCC07C67/08C07C51/02C07C51/412
Inventor 修建东
Owner 修建东
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