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High-concentration N-phenylmaleimide reaction liquid post-treatment process

A maleimide and reaction liquid technology, applied in the field of fine chemicals, can solve the problems of unmentioned yield, long overall process, affecting yield, etc., achieve rapid layering, reduce alkali consumption, and avoid three wastes Effect

Inactive Publication Date: 2016-04-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The post-processing method mentioned in CN102633706A is to cool the reaction solution to -5~0°C, and obtain the crude product N-PMI by suction filtration, then add clay and acid-binding agent to the crude product and the refined solvent, heat up and dissolve until transparent, filter and cool , crystallized and dried to obtain the product N-PMI with a purity of 99.12~99.18%, no yield mentioned
The overall process is also relatively long. Although the purity of the obtained product is high, it will affect the yield.

Method used

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  • High-concentration N-phenylmaleimide reaction liquid post-treatment process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 200ml of xylene, 13ml of dimethyl sulfoxide mixture and 160ml of water to 538g of 37.27% N-PMI reaction solution, stir at 102°C for 30min, wait for the temperature to cool to 60°C, pour 1000ml of liquid separation Layers in the funnel. When the separated aqueous phase was cooled to 20°C, it was suction-filtered in a sand core funnel with a pore size of G3 to obtain 27.4 g of 92.3% maleic anhydride solid. Pour the separated oil phase into a four-neck flask to heat, add 100g of 10% Na at 80°C 2 CO 3 Neutralize until the pH is 7, separate layers when cooled to 42°C, take the neutralized water phase for distillation, and spin the neutralized oil phase under a vacuum of -0.094Mpa to stop heating when the liquid temperature is 110°C to obtain 374.8 g solvent and 197g content are 99.25% N-PMI product, and the aftertreatment yield is 97.5%.

Embodiment 2

[0019] The operating conditions are the same as in Example 1. When washing with water, 13ml of dimethyl sulfoxide is changed to 20ml of dimethylformamide, added to 527.9g of 40% N-PMI reaction solution, stirred at 70°C for 5min, and cooled to 72°C at the same temperature When the mixture was poured into a 1000ml separatory funnel to separate layers, the rest of the conditions remained unchanged. 29.6g of 90.9% maleic anhydride solid, 380.2g of solvent and 208g of N-PMI product with a content of 99.19% were obtained, and the post-treatment yield was 97.7%.

Embodiment 3

[0021] The operating conditions are the same as in Example 1. When washing with water, 200ml of xylene is changed to 180ml of toluene and added to 529.5g of 43.3% N-PMI reaction solution, and the neutralized oil phase is subjected to spin liquid distillation at a vacuum of -0.098Mpa. The remaining conditions constant. 28.1 g of 93.5% maleic anhydride solid, 370.6 g of solvent and 226 g of N-PMI product with a content of 99.48% were obtained, and the post-treatment yield was 98.0%.

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Abstract

The invention relates to a high-concentration N-phenylmaleimide reaction liquid post-treatment process, which is uniquely characterized in that the reaction liquid is sequentially subjected to water washing and neutralization, and the obtained liquid is subjected to solvent removing in a rotary evaporator to obtain the product without re-crystallization. The process comprising: adding water and a solvent mixture to a N-phenylmaleimide reaction liquid according to a certain ratio in a mixing manner, stirring, cooling, separating to obtain a water layer and an oil layer, carrying out water washing on the water layer, cooling the washed water layer, and carrying out vacuum suction filtration to obtain a maleic anhydride (short for maleic anhydride) by-product solid and water, wherein the maleic anhydride is used as the reaction raw material so as to be continuously used for the N-phenylmaleimide reaction step, and the water is continuously used for the water washing step; carrying out water washing on the oil layer, separating the oil layer to obtain a water layer and an oil layer, and distilling the neutralization water layer to obtain water and trace residue, wherein the water is continuously used, and the residue is treated; and adding the neutralization oil layer to the rotary evaporator, and evaporating the solvent to obtain the N-phenylmaleimide finished product with the purity of more than or equal to 99.25%. According to the present invention, the yield of the whole post-treatment process can exceed 97.5%, no wastewater is generated, and the process is environmental protection.

Description

technical field [0001] The invention belongs to the field of fine chemicals and relates to a method for post-processing a high-concentration heat-resistant modifier N-phenylmaleimide reaction liquid. Background technique [0002] N-phenylmaleimide (N-PMI) is a polymer heat-resistant modifier that has emerged in recent years. It is mainly used for heat-resistant modification of ABS, PVC, PMMA resin and photosensitive materials. At present, there are a few large foreign companies producing N-PMI, such as Daihachi Chemical Company of Japan, DuPont Company of the United States, and Bayer Company of Germany, and the output in the international market is more than 80,000 tons. There are Tsinghua Unigroup, Northwest Research Institute of Chemical Industry, Hangzhou Xinyang Sanyou Chemical, Lanzhou Petrochemical and other manufacturers producing N-PMI in China. The national output is only 5,000 tons per year, and domestic products have high impurity content, impure color, short shel...

Claims

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Application Information

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IPC IPC(8): C07D207/448
Inventor 高留冕付春史乐萌孙阿沁张萍黄伟
Owner CHINA PETROLEUM & CHEM CORP
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