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Synthesis method of epoxy resin containing multiple epoxy groups

A polyepoxy-based epoxy resin and synthesis method technology, applied in the direction of organic chemistry, etc., to achieve the effects of green production process, high yield, and simple synthesis method

Active Publication Date: 2019-07-05
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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  • Synthesis method of epoxy resin containing multiple epoxy groups
  • Synthesis method of epoxy resin containing multiple epoxy groups
  • Synthesis method of epoxy resin containing multiple epoxy groups

Examples

Experimental program
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Effect test

Embodiment 1

[0026] A method for synthesizing a polyepoxy epoxy resin, comprising the following steps;

[0027] S1: Put allyl glycidyl ether and 2,3-dimercapto-1-propanol in a 2:1 molar ratio into the reactor, and add allyl glycidyl ether and 2,3-dimercapto- 1-Propanol total mass 3% of benzoin dimethyl ether and allyl glycidyl ether and 2,3-dimercapto-1-propanol 1 times the total mass of 1,4-dioxane, and put under UV lamp Under irradiation (light intensity is 10000μW / cm 2 ), reacted in an ice-water bath for 2.0 hours to obtain a reaction solution of a 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 were as follows figure 1 shown. at wavenumbers 850 and 909cm -1 The absorption peak at is the characteristic absorption peak of glycidyl ether epoxy group, and the wave number is 3450cm -1 The absorption peak at...

Embodiment 2

[0033] A method for synthesizing a polyepoxy epoxy resin, comprising the following steps;

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

[0035] S2: To the above intermediate solution, add toluene diisocyanate according to the molar ratio of toluene diisocyanate to hydroxyl group of 1.1:1, and place it at 65° C. to react for 0.5 hour. After the reaction is completed, the solvent is removed from the reaction product under the action of a rotary evaporator; the polyepoxy epoxy resin is obtained after the product is dried in a vacuum o...

Embodiment 3

[0039] A method for synthesizing a polyepoxy epoxy resin, comprising the following steps;

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

[0041] S2: in the above-mentioned intermediate solution, add diphenylmethane diisocyanate, the mol ratio of diphenylmethane diisocyanate and the intermediate is 1:1, open the stirring device, the temperature is raised to 50 ° C, and the reaction is continued for 12 hours. After the end, the solvent is removed from the reaction product under the action of a rotary evap...

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Abstract

The invention discloses an epoxy resin epoxy resin containing multiple epoxy groups, and a preparation method thereof. The method comprises the following steps: adding raw materials allyl glycidyl ether and 2,3-dimercapto-1-propanol in a reactor, adding a photoinitiator and a solvent, and carrying out a reaction in an ice water bath under ultraviolet irradiation for 1-12 h; and adding an isocyanate compound to the above obtained reaction solution, carrying out a reaction at 65 DEG C for 0.5-24 h, removing the solvent after the reaction is finished, and carrying out vacuum drying to obtain theepoxy resin containing multiple epoxy groups. The preparation method has the advantages of simplicity, high efficiency, mild reaction conditions and environmentally-friendly synthesis process.

Description

technical field [0001] The invention relates to the field of preparation methods of epoxy resins, in particular to a method for synthesizing epoxy resins containing multiple epoxy groups. Background technique [0002] Epoxy resin is one of the three major 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 polyhydric phenol and epichlorohydrin to obtain epoxy resin; 2) uses peroxyacid to convert olefinic compounds (chain or cyclic) into bismuth The bond is oxidized to an epoxy group. The epoxy resin synthesized by condensation method has high reactivity and wide application, and is the most widely used type of epoxy resin at present. However, in the synthesis process, sodium hydroxide reacts the chlorine atoms in epichlorohydrin to form sodium chloride, which needs to be removed from the epoxy resin by auxiliar...

Claims

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Application Information

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Patent Type & Authority Applications(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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