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Method for synthesizing bisphenol A diglycidyl ethers through halogen-free epoxidation

A technology of diglycidyl ether and epoxidation, which is applied in the direction of organic chemistry, etc., can solve the problems of difficult to meet the use requirements, high resin viscosity, poor product performance, etc., and achieve the effects of simple process, good product performance and easy operation.

Active Publication Date: 2013-08-14
江苏东材新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, in the synthesized bisphenol A diglycidyl ether, it is unavoidable to generate heterogeneous end groups containing organic chlorine, and at the same time, the viscosity of the resin is too high, the product performance is poor, and it is difficult to meet the use requirements.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a 1000ml four-necked flask, add 280ml chloroform, 68ml (0.222mol) bisphenol A diallyl ether, 5.48 grams (2.8×10 -3 mol) Catalyst 3, add 33.22 grams of hydrogen peroxide with a concentration of 50% (0.488mol) in the reaction flask, gradually heat and stir, react at 50°C for 8 hours, after cooling to room temperature, place in a separatory funnel After separating the organic phase and recovering chloroform by distillation, the residue was dissolved with 136 ml ethyl acetate and filtered to obtain the catalyst, and the filtrate was distilled to recover ethyl acetate to obtain a crude product. Subsequently, the product was obtained by column chromatography with a mixed solvent of petroleum ether and ethyl acetate at a volume ratio of 90:10. The product was analyzed, the epoxy equivalent test method adopted the tetraethylammonium bromide method of GB4612-84, and the viscosity (25°C, mPa.s) value was measured by the LVDV-II Brookfiel viscometer. The results are shown in Ta...

Embodiment 2

[0031] In a 1000ml four-necked flask, add 120ml 1,2-dichloroethane, 36 ml (0.1176mol) bisphenol A diallyl ether, 2.0 grams (1.1×10 -3mol) Catalyst 5, add 30.14 grams of hydrogen peroxide with a concentration of 30% (0.2660mol) in the reaction flask, gradually heat and stir, react at 80°C for 5 hours, cool to room temperature, and place in a separatory funnel After the organic phase was separated and the solvent 1,2-dichloroethane was recovered by distillation, the residue was dissolved with 60 ml of ethyl acetate and filtered to obtain the catalyst, and the filtrate was distilled to recover ethyl acetate to obtain a crude product. Subsequently, the product was obtained by column chromatography with a mixed solvent of petroleum ether and ethyl acetate at a volume ratio of 96:4. Other remaining follow-up processes are the same as in Example 1 (omitted).

Embodiment 3

[0033] Add 260ml of solvent I (dichloromethane: methyl isobutyl ketone: chloroform = 1:2:1) into a 1000ml four-neck flask, 50ml (0.1662mol) bisphenol A diallyl ether, 4.144 g (2.2×10 -3 mol) Catalyst 1, the hydrogen peroxide of 22.60 grams percent by weight concentration 50% (0.3324mol), heating gradually and stirring, reacted 12 hours under 45 ℃ of conditions, after being cooled to room temperature, separate organic phase in separatory funnel and After distilling and recovering chloroform, the residue was dissolved with 80 ml of ethyl acetate and filtered to obtain the catalyst, and the filtrate was distilled to recover ethyl acetate to obtain a crude product. Subsequently, the product was obtained by column chromatography with a mixed solvent of petroleum ether and ethyl acetate at a volume ratio of 95:5. Other remaining follow-up processes are the same as in Example 1 (omitted).

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Abstract

The invention discloses a method for synthesizing bisphenol A diglycidyl ethers through halogen-free epoxidation, which is characterized by comprising the following steps of: adding bisphenol A diallyl ethers, a solvent I and a phosphotungstic acid quaternary ammonium salt catalyst into a reactor, adding a hydrogen peroxide solution into the reactor while stirring, raising the temperature of a reactant to 30-80 DEG C, and reacting the obtained object for 5-24 hours at a temperature of 30-80 DEG C so as to obtain a reacted material; cooling the reacted material to room temperature, separating an organic phase, after the separated organic phase is subjected to distillation recycling so as to obtain an organic solvent, uniformly stirring and mixing the rest material and ethyl acetate, carrying out filtering on the obtained product, and after filter liquor is subjected to distillation recycling so as to obtain ethyl acetate, obtaining a coarse product; and carrying out column chromatography on the coarse product by using a solvent III so as to obtain bisphenol A diglycidyl ethers. After the method disclosed by the invention is adopted, no organic chlorine ion contains in the process of synthesis, a synthesized target product not only has no organochlorine heterogeneous client base, but also is low in product viscosity, good in performance, simple in process, easy to operate, high in safety, low in pollution and strong in practicability.

Description

technical field [0001] The invention belongs to the preparation of organic epoxy compounds, and relates to a method for synthesizing bisphenol A diglycidyl ether by halogen-free epoxidation. The bisphenol A diglycidyl ether prepared by the present invention is suitable for high-grade electronic components, such as casting, potting and packaging resins of light-emitting diodes (LEDs) and silicon wafers, impregnating (VPI) resins for high-grade high-voltage motors, and other application fields . Background technique [0002] Bisphenol A epoxy resin is formed by polycondensation of bisphenol A and epichlorohydrin under the action of a basic catalyst. The polycondensed bisphenol A epoxy resin is an aggregate composed of different polymerization degrees "n" values , The different values ​​of the degree of polymerization "n" lead to different forms and characteristics of epoxy resins, which can be divided into liquid and solid. Among them, bisphenol A diglycidyl ether with "n=0" ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/12C07D303/23
Inventor 吴学明杨波唐安斌李志强韩勇
Owner 江苏东材新材料有限责任公司
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