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Method for synthesizing N-phenylmaleimide and special catalyst for method

A maleimide and synthetic method technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve harsh conditions, long process and difficult operation Large and other problems, to achieve the effect of simple process, reduce the generation of waste water, and convenient operation

Active Publication Date: 2017-02-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of the catalyst is relatively long, especially the calcination temperature reaches 600°C, and the time is as long as 8 hours. The conditions are relatively harsh and the operation is difficult.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Clean the powder inside the coconut shell activated carbon with a diameter of 1~2mm with distilled water, and activate the activated carbon at 90°C for 2 hours after drying. After cooling, soak the activated carbon in 5.8 times the volume of 40% p-toluenesulfonic acid aqueous solution 24 hours, suction filtration, and drying at 130° C. for 4 hours to obtain an activated carbon-supported catalyst with an acid load of 32%, which was cooled for later use. Add activated carbon-loaded p-toluenesulfonic acid catalyst and organic solvent to the reactor at a weight ratio of 1:16, then add maleic anhydride 0.3 times the weight of the organic solvent and raise the temperature to reflux at 135°C, and continuously add maleic anhydride Add 0.8 times the mass of aniline within 2.6 hours. Keeping the reaction temperature constant for 0.8 h, the N-phenylmaleimide reaction liquid was obtained, and the yield of N-phenylmaleimide in the reaction liquid was 92%.

Embodiment 2

[0023] Use distilled water to clean the powder inside the wood activated carbon with a diameter of 1.5-3mm. After drying, activate the activated carbon at 90°C for 2 hours. Dry at 120° C. for 5 hours to obtain an activated carbon supported catalyst with an acid load of 33%, then add maleic anhydride 0.3 times the weight of the organic solvent and heat up to reflux at 135° C., continuously add aniline with 0.8 times the mass of maleic anhydride, Added within 2.6h. Keeping the reaction temperature constant for 0.8 h, the N-phenylmaleimide reaction solution was obtained, and the yield of N-phenylmaleimide in the reaction solution was 93%.

Embodiment 3

[0025] Clean the powder inside the coconut shell activated carbon with a diameter of 1~2mm with distilled water, and activate the activated carbon at 90°C for 2 hours after drying. Dry at 120°C for 5 hours to obtain an activated carbon-supported catalyst with an acid load of 36%, then add maleic anhydride 0.4 times the weight of the organic solvent and raise the temperature to reflux at 135°C, and continuously add aniline with 0.9 times the mass of maleic anhydride , Added within 2.6h. Keeping the reaction temperature constant for 1 hour, the N-phenylmaleimide reaction liquid was obtained, and the yield of N-phenylmaleimide in the reaction liquid was 95%.

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Abstract

The invention discloses a synthesis method of N-phenylmaleimide (N-PMI). Under the action of a catalyst, the N-phenylmaleimide is directly synthesized by aniline and maleic anhydride in an organic solvent; the mass ratio of the organic solvent to maleic anhydride is (0.2-0.45) to 1; the mass ratio of aniline to maleic anhydride is (0.8-0.9) to 1; the reaction temperature is 135 DEG C-140 DEG C; and the reaction time is 0.8h-1h. By adopting the method provided by the invention, wastewater can be effectively reduced; and after the reaction is finished, the amount of acid remained in an N-PMI solution is few, so that the amount of water and alkali, which are used for water washing and neutralization in a post-treatment process, can be reduced. The synthesis method is a environment-friendly process route.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for synthesizing N-phenylmaleimide and a special catalyst thereof. Background technique [0002] N-phenyl maleimide, the English name is N-phenyl maleimide, referred to as N-PMI, its molecular formula is C 16 h 7 NO 2 . N-phenylmaleimide is the simplest and one of the most important products in the rigid heat-resistant monomer N-substituent maleimide. Its appearance is light yellow flaky crystal, molecular weight 173.17, melting point 88~90℃, boiling point 162~163℃ / 1.6×10 3 Pa, hardly soluble in water, soluble in ethanol, acetone, chloroform, not very toxic to human body, but irritating to mucous membrane. [0003] Usually used in ABS, PVC, PMMA resins and photosensitive materials, it can improve the heat resistance, impact resistance, hot melt and processability of the resin, etc. It can also be used as a cross-linking agent for polypropylene...

Claims

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Application Information

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IPC IPC(8): C07D207/448B01J31/02
CPCB01J31/0225C07D207/448
Inventor 高留冕付春韦志强孙阿沁
Owner CHINA PETROLEUM & CHEM CORP
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