A kind of synthetic method of epoxy resin of many epoxy groups

A multi-epoxy epoxy resin and synthetic method technology, applied in the direction of organic chemistry, etc., to achieve the effects of mild synthesis reaction conditions, high yield, and good hydrolysis resistance

Active Publication Date: 2021-09-17
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is in order to solve the shortcoming that exists in the prior art, and proposes a kind of polyepoxide group epoxy resin and its synthetic method, the polypoxy group epoxy resin of preparation has significant compared with existing epoxy compound The toughness is improved, and no chlorine atoms are introduced, which overcomes the residual problems of organic chlorine and inorganic chlorine

Method used

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  • A kind of synthetic method of epoxy resin of many epoxy groups
  • A kind of synthetic method of epoxy resin of many epoxy groups
  • A kind of synthetic method of epoxy resin of many epoxy groups

Examples

Experimental program
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Effect test

Embodiment 1

[0026] A kind of synthetic method of epoxy resin of many epoxy groups, comprises the following steps;

[0027] S1: Put allyl glycidyl ether and 2,3-dimercapto-1-propanol in a molar ratio of 2:1 into the reactor, and add allyl glycidyl ether and 2,3-dimercapto-1-propanol 3% of the total mass of 1-propanol, benzoin dimethyl ether and allyl glycidyl ether and 1,4-dioxane of 1 times the total mass of 2,3-dimercapto-1-propanol, and in a UV lamp Under irradiation (light intensity is 10000μW / cm 2 ), reacted in an ice-water bath for 2.0 hours to obtain the reaction solution of the reaction intermediate.

[0028] The reaction solution can be concentrated on a rotary evaporator to obtain an intermediate of α-epoxy-ω-hydroxyl. Its chemical structure was characterized by infrared spectroscopy, and the results are as follows: figure 1 shown. At wavenumbers 850 and 909cm -1 The absorption peak at is the characteristic absorption peak of the glycidyl ether type epoxy group, and the wave...

Embodiment 2

[0033] A kind of synthetic method of epoxy resin of many epoxy groups, comprises the following steps;

[0034] S1: Put allyl glycidyl ether and 2,3-dimercapto-1-propanol in a molar ratio of 2.1:1 into the reactor, and add allyl glycidyl ether and 2,3-dimercapto - 3% of the total mass of 1-propanol 2-hydroxymethylphenyl propane-1-one and allyl glycidyl ether and 4 times the total mass of tetrahydrofuran of 2,3-dimercapto-1-propanol, and in UV Under lamp irradiation (light intensity is 10000μW / cm 2 ), reacted in the ice-water bath for 12 hours, and obtained the α-epoxy group-ω-hydroxyl intermediate solution after the reaction;

[0035] S2: Add toluene diisocyanate to the above intermediate solution according to the molar ratio of toluene diisocyanate to hydroxyl group 1.1:1, and react at 65°C for 0.5 hours. After the reaction is finished, the solvent is removed from the reaction product under the action of a rotary evaporator; the product is dried in a vacuum oven to obtain a ...

Embodiment 3

[0039] A kind of synthetic method of epoxy resin of many epoxy groups, comprises the following steps;

[0040] S1: Put allyl glycidyl ether and 2,3-dimercapto-1-propanol in a molar ratio of 2.5:1 into the reactor, and add allyl glycidyl ether and 2,3-dimercapto 2-methyl-1-[4-methylthiophenyl]-2-morpholino-1-propanone and allyl glycidyl ether and 2,3-dimercapto with 3% of the total mass of 1-propanol -N,N-dimethylformamide with 3 times the total mass of 1-propanol, and at 12000μW / cm 2 Under the irradiation of a special ultraviolet lamp, react in an ice-water bath for 6 hours to obtain an intermediate solution of α-epoxy-ω-hydroxyl;

[0041] S2: Add diphenylmethane diisocyanate to the above intermediate solution, the molar ratio of diphenylmethane diisocyanate to the intermediate is 1:1, turn on the stirring device, raise the temperature to 50°C, and continue the reaction for 12 hours. After the end, the solvent was removed from the reaction product under the action of a rotar...

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Abstract

The invention discloses a polyepoxy group epoxy resin and a preparation method thereof. The method puts the raw materials allyl glycidyl ether and 2,3-dimercapto-1-propanol in a reactor, and adds a photoinitiator and a solvent, and reacts 1-12 under ultraviolet light irradiation in an ice-water bath hour; then add isocyanate compound to the above reaction solution and react at 65°C for 0.5 to 24 hours, remove the solvent after the reaction, and vacuum dry to obtain a polyepoxy epoxy resin. The preparation method provided by the invention is simple and efficient, the reaction conditions are mild, and the synthesis process is environmentally friendly.

Description

technical field [0001] The invention relates to the field of preparation methods of epoxy resins, in particular to a synthesis method of epoxy resins containing multiple epoxy groups. Background technique [0002] Epoxy resin is one of the three thermosetting materials and has been widely used in coatings, adhesives and composite materials. At present, there are two main methods for synthesizing epoxy resins: 1) sodium hydroxide catalyzes the condensation of polyphenols and epichlorohydrin to obtain epoxy resins; The bonds are oxidized to epoxy groups. The epoxy resin synthesized by the condensation method has high reactivity and wide application, and is currently the most widely used type of epoxy resin. However, during the synthesis process, sodium hydroxide reacts the chlorine atoms in epichlorohydrin to generate sodium chloride, which needs to be removed from the epoxy resin through auxiliary processes such as washing, liquid separation, and drying. Otherwise, a trace...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/32C07D303/28C07D301/28
CPCC07D301/28C07D303/28C08G59/3263
Inventor 郑耀臣宋鹏赵世坤
Owner YANTAI UNIV
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