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Synthetic method of N,N'-4,4'-diphenylmethyene bismaleimide

A technology of bismaleimide and diphenylmethane, which is applied in the field of synthesis of diphenylmethane bismaleimide, can solve the problems of high cost, single reaction system, difficult wastewater treatment, etc., and achieve fast heating speed, The effect of good selectivity and high product quality

Inactive Publication Date: 2019-03-01
SHANGHAI CHEM REAGENT RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The object of the present invention is to provide a kind of synthetic method of diphenylmethane bismaleimide, synthesize diphenylmethane bismaleimide by microwave reaction, reaction system is single, easy and simple to operate, aftertreatment is simple, friendly to the environment, Overcoming the problems of high cost and difficult wastewater treatment in the preparation process of diphenylmethane bismaleimide in the prior art

Method used

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  • Synthetic method of N,N'-4,4'-diphenylmethyene bismaleimide

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Embodiment 1

[0024] A kind of synthetic method of embodiment 1 diphenylmethane bismaleimide, concrete implementation is as follows:

[0025] Maleic anhydride (9.8g, 100mmol, 99.0%), 4,4'-diaminodiphenylmethane (8.9g, 45mmol), acetic anhydride (10.7g, 105mmol), glacial acetic acid (50g, 99%) were placed In a 100mL microwave reaction tube, put it into a microwave reactor after being dissolved, set the reaction temperature to 80°C, and the reaction time to 30 minutes, turn on the microwave reactor, and stir.

[0026] After the reaction is over, transfer the reaction solution to a distillation device, distill at normal pressure, collect distillate acetic acid, add 80 g of methanol after evaporation to dryness, transfer to a reflux condensation device, reflux for 10 minutes, cool, cool to about 5°C, and suction filter, the obtained solid is 80 After vacuum drying at ℃ for 2 hours, 14.6g of a light yellow solid was obtained, i.e. the target compound diphenylmethane bismaleimide, with a purity of...

Embodiment 2

[0027] A kind of synthetic method of embodiment 2 diphenylmethane bismaleimide, concrete implementation is as follows:

[0028] Maleic anhydride (9.8g, 100mmol, 99.0%), 4,4'-diaminodiphenylmethane (9.9g, 50mmol), acetic anhydride (12.3g, 120mmol), glacial acetic acid (60g, 99%) were placed In a 100mL microwave reaction tube, put it into a microwave reactor after being dissolved, set the reaction temperature to 100°C, and the reaction time to 15 minutes, turn on the microwave reactor, and stir.

[0029] After the reaction, transfer the reaction liquid to the distillation device, distill at normal pressure, collect the distillate acetic acid, evaporate to dryness, add 98g ethanol, transfer to the reflux condensation device, reflux for 10 minutes, cool, cool down to about 5°C, and suction filter, the obtained solid is 80°C Obtain 16.5g light yellow solid after vacuum drying for 2 hours, i.e. target compound diphenylmethane bismaleimide, its purity is 98.5% (HPLC), and yield is 92...

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Abstract

A synthetic method of N,N'-4,4'-diphenylmethyene bismaleimide is provided. With maleic anhydride and 4,4'-diaminodiphenylmethane serving as raw materials, acetic anhydride as a catalyst and glacial acetic acid as a solvent, microwave reaction is carried out; N,N'-4,4'-diphenylmethyene bismaleimide is prepared then by recrystallization. The reaction in the synthetic method is simple and easy to control; posttreatment is convenient; the target product N,N'-4,4'-diphenylmethyene bismaleimide has purity of higher than 98%; the total yield is up to 90% and above; the synthetic method meets the requirements on green chemical industry.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a synthesis method of diphenylmethane bismaleimide. Background technique [0002] N,N'-4,4'-Diphenylmethane bismaleimide (BDM) is the main monomer for the synthesis of bismaleimide polymers (BMI). The main chain of BMI contains aromatic rings and nitrogen heterocyclic structures. This type of polymer has many excellent properties such as high temperature resistance, radiation resistance, friction resistance, high strength, and high weather resistance. It has been widely used in aerospace, electronics, insulating materials and other fields. . [0003] Reported in the prior art the synthesis of N, N'-(4,4'-diphenylmethane)-bismaleimide ("Henan Science" Vol.11.No.1, Mar.1993,58-63 ), using 4,4'-diaminodiphenylmethane and maleic anhydride as raw materials, acetone as solvent, metal oxide as catalyst, and N,N'-(4,4 '-diphenylmethane)-bismaleimide, the synthetic route is...

Claims

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Application Information

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IPC IPC(8): C07D207/448
CPCC07D207/448
Inventor 李海涛张传好周励詹家荣
Owner SHANGHAI CHEM REAGENT RES INST
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