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Preparing method of 3,4,3',4'-biphenyltetracarbosylic dianhydride

A technology of biphenyltetracarboxylic dianhydride and biphenyltetracarboxylic dianhydride, which is applied in the field of preparation of 3.4.3'.4'-biphenyltetracarboxylic dianhydride, can solve problems such as potential safety hazards and increase the cost of PBDA.

Inactive Publication Date: 2007-08-15
北京益利精细化学品有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The former of the above purification methods must be carried out in an autoclave, and since it is a dilute acid medium, the equipment should be a glass-lined autoclave, which has hidden dangers in terms of safety.
The latter use of expensive solvents such as dioxane will increase the cost of PBDA

Method used

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  • Preparing method of 3,4,3',4'-biphenyltetracarbosylic dianhydride
  • Preparing method of 3,4,3',4'-biphenyltetracarbosylic dianhydride
  • Preparing method of 3,4,3',4'-biphenyltetracarbosylic dianhydride

Examples

Experimental program
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Embodiment

[0040] The preparation of A, 4-chlorophthalic acid dimethyl ester:

[0041]

[0042] Add 91.2g (0.5mol) of 4-chlorophthalic anhydride, 9.1g of p-toluenesulfonic acid and 800ml of methanol into a 2000ml four-necked flask, and install a reflux condenser, a thermometer, a stirrer and a 250ml dropping funnel. Start stirring, heat the electric heating mantle to reflux, keep reflux for 4 hours, then change the reflux to distillation, every time 100ml of methanol is evaporated, add 100ml of fresh methanol from the dropping funnel, add four times like this, and finally recover all the residual methanol ( The temperature of the kettle bottle must not exceed 80°C), then turn on the water pump to pump under reduced pressure for 1 hour, vent it after cooling down, add 800ml of deionized water and stir for 5 minutes, then transfer to a 1000ml separatory funnel to stand for stratification, separate the water layer, add the oil layer After dissolving 600ml of chloroform, add 300ml of wate...

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Abstract

The invention discloses a making method of 3.4.3'.4'-biphenyl tetracarboxylic dianhydride, which comprises the following steps: adopting 4-chlorophthalandione anhydride as raw material; preparing 4-chlorophthalandione dimethyl ester, 3.3'.4.4'-biphenyl tetracarboxylic tetramethyl ester, 3.3'.4.4'-biphenyl tetracarboxylic acid and 3.3'.4.4'-biphenyl tetracarboxylic dianhydride; coupling; hydrolyzing; refining; (1) adopting p-toluenesulfonic acid as esterifying catalyst in the preparing procedure of 4-chlorophthalandione dimethyl ester; (2) adopting acetonitrile as solvent in the coupling procedure; (3) purifying hydrolytic 3.3'.4.4'-biphenyl tetracarboxylic acid through deionized water in the refining procedure; (4) washing and purifying 3.3'.4.4'-biphenyl tetracarboxylic dianhydride through acetone.

Description

technical field [0001] The present invention relates to a kind of preparation method of 3.4.3'.4'-biphenyltetraacid dianhydride. Background technique [0002] 3.4.3'.4'-Biphenyltetraacid dianhydride referred to as BPDA is an important fine chemical, which is widely used in heat-resistant polymer materials, such as a monomer for polyimide synthesis, and can also be used as a component of epoxy resin Curing agent and pharmaceutical intermediates, etc. It is most widely used in the synthesis of high temperature resistant polyimide materials. [0003] At present, only a few companies in the world produce BPDA, and the synthesis method is relatively complicated. [0004] Among the BPDA-based polyimides, the most famous one is the high-performance polyimide film - Upilex, which was successfully developed by Japan's Ube Industries Co., Ltd. in the 1980s. Since the performance of the polyimide film biphenyl is similar to that of the homophenylene polyimide film Kapton developed b...

Claims

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Application Information

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IPC IPC(8): C07D307/89
Inventor 吴俊英赵玉峰陈印山郭存林
Owner 北京益利精细化学品有限公司
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