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Method for refining and molding N-phenylmaleimide

A technology of maleimide and molding method, which is applied in the direction of organic chemistry, can solve the problems of great harm to the human body, low yield, and low content, and achieve the effects of environmental friendliness, high yield, and high content

Active Publication Date: 2013-01-02
HAISO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] N-phenylmaleimide is washed with water after the reaction, and the solvent is directly evaporated to obtain the product, which has many impurities, low content, deep color and poor stability.
However, the high-quality products obtained through recrystallization need to use organic solvents, the process is cumbersome, safety and environmental protection cannot be guaranteed, the solvent loss is large, the yield is low, and the product sublimates and volatilizes seriously during the product drying process, which is harmful to the human body. The recrystallized product is Fine powder, fluffy, easy to disperse, inconvenient to pack and use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 1000mL of toluene and 215.73g (2.2mol) of maleic anhydride to the reaction flask equipped with a thermometer, condenser, dropping funnel, and reflux separator, and start stirring. Add 186.26g (2.0mol) aniline evenly dropwise to the reaction bottle, and the dropwise addition is completed in 1-2 hours. After the dropwise addition, add 3g antioxidant hydroquinone, mixed catalyst (10g p-toluenesulfonic acid, 2g concentrated sulfuric acid ), heating to reflux until the reaction is complete, cooling down to alkali washing to neutrality, and obtaining a material-liquid organic phase containing N-phenylmaleimide.

[0019] Add 0.70g of hydroquinone to the obtained organic phase feed liquid, stir for 0.5h, remove the solvent under reduced pressure, recover 890mL of solvent, recombine the feed liquid with vacuum rectification, control the vacuum at 10mmHg, and control the feed temperature at 180°C to collect fractions 329.72g, 95.2% yield, 99.8wt% content (HPLC), 10.1g at the ...

Embodiment 2

[0021] The experiment was carried out in the same manner as in Example 1, except that the amount of stabilizer hydroquinone was changed, and 0g, 0.1g, 0.35g, 0.7g, 1.0g, 1.4g were added respectively. The experimental results are shown in Table 1.

[0022] Table 1

[0023] Adding amount of stabilizer g 0 0.10 0.35 0.70 1.0 1.4 Yield % 89.5 92.1 93.5 95.2 95.1 95.2 Contentwt% 98.5 98.9 99.4 99.8 99.8 99.7 Pan bottom wt % 10.2 6.3 5.0 2.9 3.1 2.8 color deep yellow yellow bright yellow bright yellow bright yellow bright yellow

Embodiment 3

[0025] Carry out the experiment with the same method as Example 1, the difference is to change and add different stabilizers, the addition is 0.7g, respectively with catechol, p-methoxyphenol, tert-butylcatechol, methoxybenzene Quinone was used instead of hydroquinone for experiments, and the results are shown in Table 2.

[0026] Table 2

[0027] stabilizer Catechol p-methoxyphenol tert-butylcatechol Methoxybenzoquinone Yield % 94.5 93.4 93.8 92.1 Contentwt% 99.6 99.2 99.5 99.0 Bottom wt% 3.9 5.1 4.1 6.1 color bright yellow bright yellow bright yellow bright yellow

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Abstract

The invention discloses a method for refining and molding N-phenylmaleimide. The method comprises that an N-phenylmaleimide material liquid needing refining is added with a stabilizer; the mixture is refined by a rectification technology; and a rectification fraction is processed into sheets or particles so that molding of N-phenylmaleimide is realized. The method has a product yield of 95.2% and realizes content of 99.8wt% determined by a high performance liquid chromatography (HPLC). A molded product obtained by the method is convenient for packaging and storage. The method for production of N-phenylmaleimide is environmentally friendly, has simple processes and a low cost and is convenient for large-scale industrial production.

Description

technical field [0001] The invention relates to a refining and molding method of N-phenylmaleimide. Background technique [0002] N-Phenylmaleimide (N-Phenylmaleimide) is an important organic chemical raw material with a wide range of applications. As ABS (acrylonitrile, butadiene and styrene Terpolymer ), PVC (polyvinyl chloride), PMMA (polymethyl methacrylate), PPO (polyphenylene ether) and other resin heat-resistant modifiers, can produce different types of super heat-resistant resins. It is used in antifouling coatings, heat-resistant plastics, adhesives, photosensitive resins, rubber vulcanization accelerators, insulating paints, medicines, pesticides, fungicides and antifungal agents, etc. [0003] The synthesis methods of N-phenylmaleimide mainly include one-step method, acetic anhydride method, azeotropic method and esterification method. At present, the industrialization of production at home and abroad mainly adopts the azeotropic method, which uses maleic an...

Claims

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Application Information

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IPC IPC(8): C07D207/448
Inventor 李翔刘小成邓嘉伦刘昱余丹胡雄张刚
Owner HAISO TECH
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