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Method of preparing glycidyl ether epoxy resin through monomer containing alcoholic hydroxyl group and/or phenolic hydroxyl group

A glycidyl ether and epoxy resin technology, applied in the epoxy resin field, can solve the problems of long reaction time and complicated steps, and achieve the effects of fast reaction rate, high epoxy value and mild reaction temperature

Inactive Publication Date: 2013-09-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN102153724A uses solid base as catalyst to prepare aromatic polyether glycidyl ether epoxy resin, but has the disadvantage of long reaction time (5-20 hours)
Patent US5420312A discloses a method for preparing glycidyl ether from alcohol and epichlorohydrin. Using a three-step or two-step method, cyclohexanedimethanol diglycidyl ether with an epoxy value of 0.691 can be prepared. This method The steps are more complicated (the last step of the reaction requires vacuuming), and the reaction time is longer

Method used

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  • Method of preparing glycidyl ether epoxy resin through monomer containing alcoholic hydroxyl group and/or phenolic hydroxyl group
  • Method of preparing glycidyl ether epoxy resin through monomer containing alcoholic hydroxyl group and/or phenolic hydroxyl group
  • Method of preparing glycidyl ether epoxy resin through monomer containing alcoholic hydroxyl group and/or phenolic hydroxyl group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In a 250mL four-neck flask equipped with a stirring paddle, a thermometer, a condenser, and a nitrogen conduit, add 31.2g of bisphenol A polyoxyethylene ether (BAEO-2) with the following structure and 95g of epichlorohydrin. The system was heated up to 56°C and stirred to fully dissolve the raw materials in epichlorohydrin, then 0.25g of tetramethylammonium bromide and 14g of granular solid sodium hydroxide were added to start timing. During the reaction, the temperature of the system will rise. At this time, use a cold water bath to maintain the reaction system at 56±2°C. When the temperature begins to drop, heat and keep the system at 56±2°C again. After 2.5 hours, the reaction was stopped, and the salt and unreacted base generated by the reaction were removed by suction filtration. Pour the filtrate into a 500mL separatory funnel, add about 130mL of toluene to dilute, and wash the product with deionized water until neutral, then separate the organic phase. Under the...

Embodiment 2

[0042] In a 250mL four-necked flask equipped with a stirring paddle, a thermometer, a condenser, and a nitrogen conduit, 36.6g of bisphenol A polyoxyethylene ether BAEO-2 and 51.2g of epichlorohydrin were added. The system was heated up to 56° C. and stirred to fully dissolve the raw materials in epichlorohydrin, and then 0.3 g of tetramethylammonium bromide and 16.5 g of granular solid sodium hydroxide were added to start timing. Adopt the method of embodiment 1 to control reaction temperature to be 56 ± 2 ℃. After 2.5 hours, the reaction was stopped, and the salt and unreacted base generated by the reaction were removed by suction filtration. Pour the filtrate into a 500mL separatory funnel, add about 150mL of toluene to dilute, and wash the product with deionized water until neutral, then separate the organic phase. Under the pressure of 1-10mmHg, the volatile matter in the organic phase is distilled out by stepwise temperature rise from 60°C to 135°C, and the epoxy value ...

Embodiment 3

[0044]In a 250mL four-necked flask equipped with a stirring paddle, a thermometer, a condenser, and a nitrogen conduit, 31.5g of bisphenol A polyoxyethylene ether BAEO-2 and 94.5g of epichlorohydrin were added. The system was heated up to 56°C and stirred to fully dissolve the raw materials in epichlorohydrin, then 0.26g of tetramethylammonium bromide and 9.5g of granular solid sodium hydroxide were added to start timing. Adopt the method of embodiment 1 to control reaction temperature to be 56 ± 2 ℃. After 2.5 hours, the reaction was stopped, and the salt and unreacted base generated by the reaction were removed by suction filtration. Pour the filtrate into a 500mL separatory funnel, add about 130mL of toluene to dilute, and wash the product with deionized water until neutral, then separate the organic phase. Under the pressure of 1-10mmHg, the volatile matter in the organic phase is distilled out by stepwise temperature rise from 60°C to 135°C, and the epoxy value of the ob...

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Abstract

The invention discloses a method of preparing glycidyl ether epoxy resin through monomer containing alcoholic hydroxyl group and / or phenolic hydroxyl group, belonging to the technical field of epoxy resin. The method comprises the following steps of: adding the monomer containing alcoholic hydroxyl group and / or phenolic hydroxyl group and epoxy chloropropane into a reactor, and heating the reactor to fully dissolve the ingredients; controlling the reaction temperature to 40-80 DEG C, and adding a quaternary ammonium salt and solid alkali; pumping and filtering to remove the redundant alkali and the generated salt after the reaction is finished for 0.5-5 hours, adding an organic solvent immiscible to water while capable of dissolving the obtained epoxy resin to dilute the product, washing the product through deionized water for multiple times, separating out an organic phase, and decompression distilling. The method provided by the invention has the advantages of high reaction speed, high percent conversion and capable of simultaneously etherifying the alcoholic hydroxyl group and the phenolic hydroxyl group.

Description

technical field [0001] The invention relates to a method for preparing glycidyl ether epoxy resin from monomers containing alcoholic and / or phenolic hydroxyl groups, and belongs to the technical field of epoxy resins. Background technique [0002] The corresponding glycidyl ether epoxy resin can be prepared by reacting alcoholic or phenolic hydroxyl-containing monomers with epichlorohydrin. However, there are differences in the reactivity of alcoholic hydroxyl groups and phenolic hydroxyl groups with epichlorohydrin: in the etherification reaction process of alcoholic hydroxyl groups and epichlorohydrin, Lewis acids (such as BF 3 ·OEt 2 ) as a catalyst for the ring-opening reaction, but the catalytic effect of the catalyst on the ring-opening reaction of phenolic hydroxyl and epichlorohydrin is not obvious; the reaction between phenolic hydroxyl and epichlorohydrin can use sodium hydroxide solution as the ring-opening reaction and final ring-closing The catalyst for the re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/04
Inventor 程珏樊孟金张军营李相元
Owner BEIJING UNIV OF CHEM TECH
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