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Preparation method of chlorendic anhydride

The technology of chloro bridged acid anhydride and maleic anhydride is applied in the field of preparation of chlorine-based flame retardant chloro bridge acid anhydride, which can solve the problems of complicated crystallization process with hot water and dilute acetic acid, long reaction time, low yield and the like, and achieve white color. , The effect of short reaction time and high yield

Active Publication Date: 2015-06-17
JIANGSU ANPON ELECTROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction time is long, tar-like impurities are produced, the crystallization process with hot water and dilute acetic acid is complicated, and the investment is large
The yield of this method is low, which can only reach about 70%, and the cost is high; the obtained product must be refined twice before it can be used for polyester production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 273 grams (1mol) of hexachlorocyclopentadiene into a 250ml four-necked flask with a stirrer and a thermometer, raise the temperature, add 99 grams of maleic anhydride (1.01mol) dropwise, and control the temperature at 160~170°C for 2 hours Then add 15 grams of chlorobenzene, continue the reaction for 2 hours, cool down to end the reaction, filter with suction and dry to obtain 359 grams of white chlorobridge anhydride, the content is 99.2%, and the yield is 96%.

Embodiment 2

[0019] Add 273 grams (1mol) of hexachlorocyclopentadiene (1mol) and 12 grams of toluene to a 250ml four-necked flask with a stirrer and a thermometer, raise the temperature, add 99 grams of maleic anhydride (1.01mol), and control the temperature at 160~170°C after adding , reacted for 5 hours, cooled to end the reaction, suction filtered and dried to obtain 351 grams of white chlorobridge anhydride, with a content of 98.4% and a yield of 94%.

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Abstract

The invention discloses a preparation method of chlorendic anhydride. The chlorendic anhydride is prepared through a reaction of maleic anhydride and hexachlorocyclopentadiene. According to the invention, maleic anhydride is added into hexachlorocyclopentadiene, wherein a molecular ratio of maleic anhydride to hexachlorocyclopentadiene is (1-1.05):(1-1.05). A diluting agent should be added before or during the reaction. The reaction temperature is 150-180 DEG C, and a reaction time is 2-5h. According to the invention, maleic anhydride is added into hexachlorocyclopentadiene, and a reaction is carried for 2-5h under a temperature of 150-180 DEG C, such that high-quality chlorendic anhydride is successfully produced, and a yield reaches 96%. The chlorendic anhydride can be directly used in polyester production. The method has the advantages such as easy-to-obtain raw materials, short reaction time, simple operation, low investment, and high yield.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a preparation method of chlorine-based flame retardant chlorobridge anhydride. Background technique [0002] Chlorendic anhydride English name Chlorendic anhydride, CAS115-27-5, is a white crystal, suitable for unsaturated polyester, polyurethane and epoxy resin, also used as epoxy resin curing agent. The heat distortion temperature of epoxy resin products cured by this product is about 180 ℃, and it has good drug resistance. Chlorbridge acid is also used as a dye intermediate and insecticide. It is also used as a flame retardant for fabrics. It is usually obtained by reacting hexachlorocyclopentadiene with maleic anhydride. Mix hexachlorocyclopentadiene and maleic anhydride in the solvent chlorobenzene at a molar ratio of 1:1.1, react at 140-145°C for 7-8 hours, add the reaction product into water for hydrolysis, and hydrolyze the obtained chlorine at 70°C Bridge ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/00
Inventor 季玉祥姜育田陈灿银宋静德程恒洲王朝会
Owner JIANGSU ANPON ELECTROCHEM
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