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Method for preparing recyclable epoxy resin by utilizing ontology click chemistry reaction

A click chemical reaction and epoxy resin technology, applied in the field of thermoplastic epoxy resin and its preparation, can solve the problems of slow reaction rate of amine and epoxy, reaction conversion rate cannot reach 100%, harsh reaction conditions, etc., and the method is simple and convenient. , Superior mechanical properties, toughness enhancement effect

Active Publication Date: 2018-07-20
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its existing technical defects are: the reaction rate of amine and epoxy is relatively slow, the reaction conditions are relatively harsh, and the reaction conversion rate cannot reach 100%, which is mentioned in the literature as 94%

Method used

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  • Method for preparing recyclable epoxy resin by utilizing ontology click chemistry reaction
  • Method for preparing recyclable epoxy resin by utilizing ontology click chemistry reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1, a kind of preparation method of reusable epoxy resin, polyfunctional epoxy resin selects novolac epoxy resin, tertiary amine catalyst selects N,N-dimethylbenzylamine, and carries out the following steps successively:

[0030] 1) In a constant temperature oil bath at 20°C, add 40g of novolac epoxy resin and 16g of furfuryl mercaptan into a 100ml three-neck round bottom flask, and mix well by mechanical stirring; then add 1g of N,N-dimethylbenzyl The amine was placed in a nitrogen protective atmosphere and reacted for 3 hours to obtain an intermediate whose terminal group was a furan functional group, and the grafting rate reached 99.9%.

[0031] 2) Under the protection of nitrogen, the intermediate obtained by the reaction and 45g of N-N'-(4,4-methylenediphenyl)bismaleimide were stirred evenly in a constant temperature oil bath at 160°C, Fully react for 0.1 hour, pour into a polytetrafluoroethylene mold placed in an oven, and carry out crosslinking reaction...

Embodiment 2

[0032] Embodiment 2, a kind of preparation method of reusable epoxy resin, polyfunctional epoxy resin selects triglycidyl p-aminophenol, three (4-hydroxyphenyl) methane triglycidyl ether and 2,2 ', 2",2"'-[1,2-bis-dimethylene tetrakis(4,1-phenylene methylene oxide)]tetraoxirane mixture, bis(2-dimethyl Aminoethyl) ether, the steps are as follows:

[0033] 1) In a constant temperature oil bath at 100°C, add 22g of triglycidyl p-aminophenol, 10g of tris(4-hydroxyphenyl)methane triglycidyl ether and 38g of 2,2',2",2"' Add -[1,2-bidimethylene tetrakis(4,1-phenylene methylene oxide)]tetraoxirane and 33g furfuryl mercaptan into a 150ml three-neck round bottom flask, and mix well by mechanical stirring . Then 2.1 g of bis(2-dimethylaminoethyl) ether was added, placed in a nitrogen atmosphere, and reacted for 0.1 hour to obtain an intermediate whose terminal group was a furan functional group, and the grafting rate reached 99.7%.

[0034] 2) Under the protection of nitrogen, the int...

Embodiment 3

[0035] Embodiment 3, a kind of preparation method of reusable epoxy resin, multifunctional epoxy resin selects 1,1,1-three (4-hydroxyphenyl) ethyl triglycidyl ether and 4,4'-diamino The mixture of diphenylmethane epoxy resin, tertiary amine catalyst selects triethylamine for use, and step is as follows:

[0036] 1), in a constant temperature oil bath at 40°C, mix 22g of 1,1,1-tris(4-hydroxyphenyl)ethyl triglycidyl ether and 23g of 4,4'-diaminodiphenylmethane epoxy resin with 40g Furfuryl mercaptan was added into a 150ml three-necked round-bottomed flask, and mixed evenly by mechanical stirring. Then 2 g of triethylamine was added, placed in a nitrogen atmosphere, and reacted for 2 hours to obtain an intermediate whose terminal group was a furan functional group, and the grafting rate reached 99.8%.

[0037] 2), under the protection of nitrogen, the intermediate obtained by the reaction and 42g of N-N-(4-methyl-1,3-phenylene)bismaleimide were stirred evenly in a constant tempe...

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Abstract

The invention relates to a thermoplastic epoxy resin with thermal reversible chemical crosslinking property and a preparation method thereof and in particular relates to a method for preparing a recyclable epoxy resin by utilizing an ontology click chemistry reaction. The method comprises the following steps: 1) carrying out a click reaction on multifunctional epoxy resin and furfurylmercaptan inthe presence of a tertiary amine catalyst so as to obtain an intermediate of which the end group is a furan functional group; 2) carrying out a Diels-Alder reaction on the intermediate and a cross-linking agent containing a maleimide group, thereby obtaining the reversible crosslinking epoxy resin. According to the method disclosed by the invention, the defect that the traditional cured epoxy resin is refractory is overcome, so that the epoxy resin can realize decrosslinking at a high temperature, so that recycling and secondary processing of the epoxy resin can be realized.

Description

technical field [0001] The invention relates to a thermoplastic epoxy resin with thermoreversible chemical crosslinking properties and a preparation method thereof, in particular to a method for preparing reusable epoxy resin by bulk click chemical reaction. Background technique [0002] Epoxy resin is an important thermosetting polymer, which is widely used in adhesives, structural materials, printed circuit boards, electronic packaging and other fields due to its strong chemical stability, low shrinkage, and high dielectric properties. Traditional covalently cross-linked epoxy resins are brittle due to their high cross-linking density, which limits their applications. Moreover, due to the irreversibility of the crosslinking reaction, the cured epoxy resin is difficult to be reprocessed by some methods such as heat treatment, which limits its repeated recycling and causes a large waste of resources. [0003] There have been many studies on the toughening modification based...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/32C08G59/66C08G59/68
CPCC08G59/3218C08G59/3227C08G59/66C08G59/686
Inventor 姚臻于云飞王建斌曹堃
Owner ZHEJIANG UNIV
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