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A kind of synthetic method of linear epoxy resin containing multiple glycidyl ether groups

A glycidyl ether-based, linear epoxy resin technology, applied in the field of online epoxy resin synthesis, can solve difficult problems and achieve excellent alkali resistance and high reactivity

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

AI Technical Summary

Problems solved by technology

[0006] However, the distance between two adjacent epoxy groups in the epoxy resin molecular structure (or the density / distribution of epoxy groups in the epoxy resin) can only be regulated by changing the molecular weight of the dimercapto compound. Dimercapto compounds containing more than sixteen carbon atoms (1,16-dimercaptohexadecane) are very difficult
Therefore, the idea of ​​greatly adjusting the properties of crosslinked materials by adjusting the density or distribution of epoxy groups in epoxy resins cannot be realized by existing synthetic routes.

Method used

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  • A kind of synthetic method of linear epoxy resin containing multiple glycidyl ether groups
  • A kind of synthetic method of linear epoxy resin containing multiple glycidyl ether groups
  • A kind of synthetic method of linear epoxy resin containing multiple glycidyl ether groups

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Experimental program
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Embodiment 1

[0044] Embodiment 1-4 is the specific implementation example of reaction after mixing propargyl glycidyl ether and propargyl methyl ether in different molar ratios, wherein the molar ratio of the two in embodiment 1 is 1:1, and in embodiment 2, two The molar ratio of the two is 2:1, the molar ratio of the two is 1:2 in embodiment 3, and the molar ratio of the two is 1:4 in embodiment 4.

[0045] Example 1

[0046] A method for synthesizing a linear epoxy resin containing multiple glycidyl ether groups, comprising the following steps;

[0047] S1: Mix the raw material propargyl glycidyl ether and propargyl methyl ether according to the molar ratio of 1:1, and then react with the raw material 1,5-pentanedithiol according to the molar ratio of alkynyl and mercapto groups of 1:2 In the container, add the benzoin dimethyl ether of 5% of the total mass of the raw materials and the 1,4-dioxane of 200% of the total mass of the raw materials, in an ice-water bath, ultraviolet light ir...

Embodiment 2

[0058] A synthetic method of a linear epoxy resin containing multiple glycidyl ether groups, the synthetic method is the same as in Example 1, the difference is that in step S1 the raw material propargyl glycidyl ether and propargyl methyl ether are in a molar ratio of 2 :1 mix.

[0059] The structure of the product (linear epoxy resin containing multiple glycidyl ether groups) obtained in embodiment 2 has been characterized with nuclear magnetic resonance spectrum, see Figure 6 . The chemical shifts of hydrogen protons in different chemical environments in the product of Example 2 have been assigned, and have been marked in the spectrogram, such as Figure 6 Shown in (a), the absorption peak at chemical shift 2.5-3.2ppm is the chemical shift of hydrogen on the epoxy group, as Figure 6 As shown in (b), the corresponding chemical shifts in the carbon nuclear magnetic spectrum appear at 44.2ppm and 50.9ppm respectively, indicating that the epoxy group has successfully entere...

Embodiment 3

[0066] A kind of synthetic method of the linear epoxy resin that contains a plurality of glycidyl ether groups, synthetic method is the same as embodiment 1, difference is that in step S1 raw material propargyl glycidyl ether and propargyl methyl ether according to molar ratio 1 :2 mixed.

[0067] The structure of the product (linear epoxy resin containing multiple glycidyl ether groups) obtained in embodiment 3 has been characterized by nuclear magnetic resonance spectrum ( Figure 8 ), indicating that the epoxy group has successfully entered the structure of the copolymerization product and proves that the mercapto-alkyne copolymerization reaction adopted in this example is successful.

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Abstract

The invention discloses a linear epoxy resin containing multiple glycidyl ether groups and a preparation method thereof. In the method, propargyl glycidyl ether, propargyl ether (or alkyl-1-alkyne) and dimercapto compound are placed in a reactor, and a catalyst and a solvent are added, and react under ultraviolet light irradiation in an ice-water bath 1.0-6.0 hours; then add allyl glycidyl ether and catalyst to the above-mentioned reaction solution and continue to react for 0.5-3.0 hours, after the reaction finishes, remove the solvent and unreacted raw materials by precipitation, and vacuum dry to obtain a compound containing multiple Linear epoxy resin with glycidyl ether groups. 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 linear epoxy resins containing multiple glycidyl ether groups. Background technique [0002] Epoxy resin is a kind of thermoplastic oligomer containing two or more epoxy groups. Because its molecular structure contains highly reactive epoxy groups, epoxy resin can be used as the main matrix and is widely used in coatings. , adhesives or multiple fields of composite materials. [0003] At present, there are two main routes for the preparation of polyepoxide-based linear epoxy resins: [0004] 1) Using glycidyl methacrylate (GMA) as a raw material, free radical polymerization (including controlled free radical polymerization, such as atom transfer radical polymerization or reversible addition-fragmentation chain transfer polymerization) or free radical copolymerization, The corresponding linear polyglycidyl methacrylate (PGMA) or a linear c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/02C08G59/32
CPCC08G59/022C08G59/027C08G59/3263
Inventor 郑耀臣宋鹏张谦刘健赵世坤
Owner YANTAI UNIV
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