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Method for preparing maleimide-containing epoxy resin curing agent

A technology of maleimide epoxy resin and curing agent, which is applied in organic chemistry and other fields, and can solve the problems of unseen modified product reports and patents

Inactive Publication Date: 2015-04-22
CHENGDU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0033] Have not yet seen any reports and patents of novel epoxy resins and coatings thereof prepared by glycidyl epoxy resin curing agents containing maleimide structures, nor have any reports and patents of this new material and other resin modified products Reports and patents (see attached novelty search report)

Method used

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  • Method for preparing maleimide-containing epoxy resin curing agent
  • Method for preparing maleimide-containing epoxy resin curing agent
  • Method for preparing maleimide-containing epoxy resin curing agent

Examples

Experimental program
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Effect test

Embodiment 1

[0049] In the present embodiment, the preparation method that contains maleimide epoxy resin curing agent, its processing step is as follows successively:

[0050] (1) After dissolving 20.2g of N-(4-aminophenyl)maleimide and 0.25g of phase transfer catalyst benzyltriethylammonium chloride with 300ml of absolute ethanol, under the condition of nitrogen protection, the temperature was raised to 65°C, and then dropwise added 24.9 g of epichlorohydrin, and after the dropwise addition, the temperature was lowered to 55°C and reacted for 5 hours.

[0051] (2) Cool the reaction system to 30-40° C. and add 8.6 g of solid sodium hydroxide, then raise the temperature to 50° C. for 3 hours for ring closure reaction.

[0052] (3) After the reaction, cool down to room temperature, filter with suction, extract the filtrate with 3000ml of ethyl acetate, wash with deionized water for 3 times, and remove the ethyl acetate by rotary evaporation at 45°C to obtain the brown viscous target Produc...

Embodiment 2

[0054] In the present embodiment, the preparation method that contains maleimide epoxy resin curing agent, its processing step is as follows successively:

[0055] (1) After dissolving 20.2g of N-(4-aminophenyl)maleimide and 0.25g of phase transfer catalyst tetrabutylammonium chloride in 300ml of propanol, the temperature was raised to 65°C under nitrogen protection , and then 24.9 g of epichlorohydrin was added dropwise, and after the dropwise addition, the temperature was lowered to 55° C. and reacted for 4 hours.

[0056] (2) Cool the reaction system to 30-40°C and add 8.6g of solid sodium hydroxide, then raise the temperature to 50°C to carry out the ring-closing reaction for 4 hours.

[0057] (3) After the reaction, cool down to room temperature, filter with suction, extract the filtrate with 4200ml of ethyl acetate, wash with deionized water for 3 times, and remove the ethyl acetate by rotary evaporation at 45°C to obtain the brown viscous target Product—contains maleim...

Embodiment 3

[0059] In the present embodiment, the preparation method that contains maleimide epoxy resin curing agent, its processing step is as follows successively:

[0060] (1) After dissolving 20.2g of N-(4-aminophenyl)maleimide, 0.25g of phase transfer catalyst benzyltriethylammonium chloride with 360ml of absolute ethanol, under the condition of nitrogen protection, the temperature was raised After reaching 65°C, 29.9 g of epichlorohydrin was added dropwise, and after the dropwise addition, the temperature was lowered to 55°C and inverted for 6 hours.

[0061] (2) The temperature of the reaction system was lowered to 30-40° C. and 8.6 g of solid potassium hydroxide was added, and then the temperature was raised to 50° C. for 2 hours of ring closure reaction.

[0062] (3) After the reaction, cool down to room temperature, filter with suction, extract the filtrate with 3000ml of ethyl acetate, wash with deionized water for 3 times, and remove the ethyl acetate by rotary evaporation at...

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Abstract

The invention belongs to the field of epoxy resin curing agents, and in particular relates to a method for preparing a maleimide-containing epoxy resin curing agent. The method for preparing the maleimide-containing epoxy resin curing agent is simple and environment-friendly in process, wide in reaction temperature range, gentle in reaction condition and beneficial to industrial production. The method comprises the following process steps in sequence: (1) dissolving an amine compound and a phase transferring catalyst into a proper amount of organic solvent; under the protection of nitrogen, heating to 65 DEG C, then dropwise adding epoxy chloropropane; and after epoxy chloropropane is completely dropwise added, cooling to 55 DEG C, reacting for 2-8 hours; (2) cooling the reaction system to 30-40 DEG C, adding solid alkali, heating to 50 DEG C, and implementing ring-closure reaction for 1-6 hours; (3) cooling to the room temperature after the reaction is finished, performing suction filtration, extracting the filtrate by using a proper amount of ethyl acetate, washing with deionized water for many times, and implementing rotary evaporation at 45 DEG C so as to remove ethyl acetate, thereby obtaining a target product, namely maleimide-containing epoxy resin curing agent.

Description

Technical field: [0001] The invention belongs to the field of preparation of epoxy resin curing agent, in particular to a preparation method of maleimide-containing epoxy resin curing agent. Background technique: [0002] Epoxy resin is a kind of oligomeric molecule formed by ring-opening reaction of epoxy group with aromatic, aliphatic or alicyclic carbon bond as the skeleton containing two or more epoxy groups. things. It has liquid, solid, viscous and other forms, and it has almost no application value when used alone. It must be added with a curing agent to form a three-dimensional network structure before it can become an epoxy material with various excellent properties. Epoxy resin has good dielectric properties, small shrinkage rate of products, good stability, strong adhesion to metal and non-metal materials, high hardness and good flexibility, and good stability to most solvents and lyes. It is widely used in electronics, machinery, construction, aerospace and oth...

Claims

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Application Information

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IPC IPC(8): C07D405/14C08G59/40
CPCC07D405/14C08G59/4042
Inventor 陶果肖蔓杨帆常波张琦
Owner CHENGDU NORMAL UNIV
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