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Method for preparing 3,3',4,4'-benzophenonetetracarboxylic dianhydride

A technology of benzophenone tetraacid dianhydride and o-xylene, which is applied in the field of organic synthesis, can solve the problems of complex process, cannot meet domestic demand, small production scale, etc., and achieves a simple process, easy industrialization implementation, and low production cost. Effect

Active Publication Date: 2014-03-12
六安科瑞达新型材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Domestic scientific research institutions have also carried out synthetic research and trial production of ketone anhydride. The current process is complicated and the production scale is small, which cannot meet domestic demand.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Feed molar ratio: o-xylene, bis(trichloromethyl)carbonate=10:1.0, Lewis acid is aluminum trichloride, the dosage is 3.1 times of bis(trichloromethyl)carbonate; high manganese The molar ratio of potassium dichloride to bis(3,4-xylyl)methanone is 4:1, and the dosage of 0.10mol / L hydrochloric acid solution is 400ml.

[0020] (1). Add 124.74 g (0.42 mol) of bis(trichloromethyl)carbonate and o Toluene 507mL (4.20mol), under the protection of nitrogen, control the temperature at 3-5°C, stir for 2h; then put in finely ground aluminum chloride 173.82g (1.30mol) and stir to make it uniform, 0-5°C heat preservation reaction After 4 hours, 500ml of water was added to the four-necked flask, and the temperature was raised to 40°C with stirring, and the reaction was kept for 2 hours. After the reaction was completed, the solid aluminum hydroxide was removed by filtration, and the filtrate was separated into an organic phase with a separatory funnel. The organic phase was distilled ...

Embodiment 2

[0024] Feed molar ratio: o-xylene, bis(trichloromethyl)carbonate=10:1.0, Lewis acid is aluminum trichloride, the dosage is 3.3 times of bis(trichloromethyl)carbonate; high manganese The molar ratio of potassium dichloride to bis(3,4-xylyl)methanone is 5:1, and the dosage of 0.10mol / L hydrochloric acid solution is 500ml.

[0025] (1). Add 124.74 g (0.42 mol) of bis(trichloromethyl)carbonate and o-dicarbonate into a 2000ml four-necked flask equipped with a mechanical stirrer, a thermometer and a condenser tube equipped with an anhydrous calcium chloride drying tube on the upper end. Toluene 507mL (4.20mol), under the protection of nitrogen, control the temperature at 0-2°C, stir the reaction for 3h, put in the finely ground aluminum chloride 185.57g (1.39mol) and stir to make it uniform, keep the reaction at 0-5°C After 6 hours, add 600ml of water into the four-necked flask and stir to raise the temperature to 40°C, keep the temperature for 2 hours, and after the reaction is com...

Embodiment 3

[0029] Feed molar ratio: o-xylene, bis(trichloromethyl)carbonate=12:1.0, Lewis acid is aluminum trichloride, the dosage is 3.5 times of bis(trichloromethyl)carbonate; high manganese The molar ratio of potassium bis(3,4-xylyl)methanone to bis(3,4-xylyl)methanone is 4.5:1, and the dosage of 0.10mol / L hydrochloric acid solution is 600ml.

[0030](1). Add 124.74 g (0.42 mol) of bis(trichloromethyl)carbonate and o Toluene 608mL (5.04mol), under the protection of nitrogen, the temperature was controlled at 0-2°C, and the reaction was stirred for 3h. Then put in 196.25g (1.47mol) of finely ground aluminum chloride and stir to make it uniform. After 5 hours of heat preservation at 0-5°C, add 600ml of water into the four-necked flask and stir to raise the temperature to 40°C, and heat the reaction for 2 hours. After the reaction was completed, the solid aluminum hydroxide was removed by filtration, and the filtrate was separated into an organic phase with a separatory funnel. The org...

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Abstract

The invention discloses a method for synthesizing 3,3',4,4'-benzophenonetetracarboxylic dianhydride by taking o-xylene and bis(trichloromethyl) carbonate as raw materials. The method comprises the steps of: by taking o-xylene and bis(trichloromethyl) carbonate as the raw materials, performing acylation reaction in catalysis of anhydrous lewis acid, thus obtaining bis(3,4-ditolyl)methanone; fully oxidizing bis(3,4-ditolyl)methanone in a potassium permanganate / hydrochloric acid system, and carrying out filtration, concentration, crystallization and the like to obtain 3,3',4,4'-benzophenonetetracarboxylic acid; performing vacuum high-temperature melting and dehydration to 3,3',4,4'-benzophenonetetracarboxylic acid to obtain the 3,3',4,4'-benzophenonetetracarboxylic dianhydride product. The preparation method has the advantages of being simple in technology, high in yield, fewer in three wastes, capable of recycling anhydrous lewis acid, low in production cost and easy for industrial implementation, and the like.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of 3,3',4,4'-benzophenonetetraacid dianhydride. Background technique [0002] 3,3',4,4'-Benzophenonetetraacid dianhydride, referred to as ketone anhydride (BTDA), is an important raw material for the synthesis of polyimides. At present, ketone anhydride polyimides are mainly used as compound The matrix resin of the material has a wide range of temperature resistance, excellent corrosion resistance, radiation resistance, insulation, impact resistance, etc., and can be made into structural parts, laminates, films, adhesives, coatings, insulating materials and reinforcement materials, etc. , Widely used in aviation / aerospace, electrical / electronics, ships, automobiles, precision machinery and other fields. The development of p-ketone anhydride in foreign countries began in the 1960s. The main unit engaged in research and production is the Gulf Petrochemical Co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/89
CPCC07D307/89
Inventor 鲍远志翁世兵柴多里
Owner 六安科瑞达新型材料有限公司
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