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Preparation method for biphenyltetracarboxylic dianhydride mixture

A biphenyl dianhydride and mixture technology, which is applied in the field of preparing biphenyl dianhydride mixtures, can solve the problems of low efficiency and high cost, and achieve the effects of low cost, increased efficiency, and reduced cost

Inactive Publication Date: 2016-02-17
苏州亚培克生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The single reaction route product of the above method has only one isomer, which has low efficiency and high cost

Method used

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  • Preparation method for biphenyltetracarboxylic dianhydride mixture
  • Preparation method for biphenyltetracarboxylic dianhydride mixture
  • Preparation method for biphenyltetracarboxylic dianhydride mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dissolve phthalic acid (1 mmol) in 20 ml of aqueous acid solution, stir for 1.5 hours, pass chlorine gas into it, react for 3 hours, drain all solvents, add 50 ml of ethyl acetate, and wash the resulting solution with saturated brine for 3 After separation of the organic phase, the aqueous phase was extracted twice with ethyl acetate (50 mL). The organic phases were combined, dried with a desiccant, filtered off the desiccant, and evaporated to dryness to obtain the corresponding ortho- and meta-substituted phthalic acid chlorides (yield 100%, GC purity (two isomers) 99 %).

[0032] Dissolve phthalic acid chloride (1 mmol) in 20 ml of methanol, add alkali solution, stir for 1.5 hours, drain all solvents, add 50 ml of ethyl acetate, wash the resulting solution 3 times with saturated brine, and remove the organic phase After separation, the aqueous phase was extracted twice with ethyl acetate (50 mL). The organic phases were combined, dried with desiccant, filtered off ...

Embodiment 2

[0036] 1 Dissolve phthalic acid (1 mmol) in 20 ml of aqueous acid solution, stir for 1.5 hours, pass bromine gas into it, react for 3 hours, drain all solvents, add 50 ml of ethyl acetate, and wash the resulting solution with saturated salt After washing with water three times, the organic phase was separated, and the aqueous phase was extracted twice with diethyl ether (50 mL). The organic phases were combined, dried with a desiccant, filtered off the desiccant, and evaporated to dryness to obtain the corresponding ortho- and meta-substituted phthalic acid chlorides (yield 100%, GC purity (two isomers) 98 %).

[0037] Dissolve phthalic acid chloride (1 mmol) in 22 ml of isopropanol, add alkali solution, stir for 1.5 hours, drain all the solvent, add 50 ml of ether, wash the resulting solution 3 times with saturated saline, and the organic phase After separation, the aqueous phase was extracted twice with ether (50 mL). The organic phases were combined, dried with desiccant,...

Embodiment 3

[0041] Dissolve phthalic acid (1 mmol) in 20 ml of aqueous acid solution, stir for 1.5 hours, pass bromine gas into it, react for 3 hours, drain all solvents, add 50 ml of ethyl acetate, and wash the resulting solution with saturated saline 3 times, after separation of the organic phase, the aqueous phase was extracted twice with dichloromethane (50 mL). The organic phases were combined, dried with a desiccant, filtered off the desiccant, and evaporated to dryness to obtain the corresponding ortho- and meta-substituted phthalic acid chlorides (yield 100%, GC purity (two isomers) 99 %).

[0042] Dissolve phthalic acid chloride (1 mmol) in 25 ml of ethanol, add alkali solution, stir for 1.5 hours, drain all solvents, add 50 ml of dichloromethane, and wash the resulting solution 3 times with saturated brine, and the organic phase After separation, the aqueous phase was extracted twice with dichloromethane (50 mL). The organic phases were combined, dried with desiccant, filtered...

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Abstract

The invention relates to a preparation method for a biphenyltetracarboxylic dianhydride mixture. The preparation method comprises the following steps: with phthalic acid as a starting raw material, carrying out an electrophilic substitution reaction so as to produce a phthalic acid derivative; then subjecting the derivative to esterification so as to produce phthalate; further catalyzing phthalate and carrying out a coupling reaction so as to produce a biphenyl tetraformate mixture; and finally, successively carrying out saponification and acidification so as to produce the product biphenyltetracarboxylic dianhydride mixture. The method provided by the invention uses cheap and easily phthalic acid as the starting raw material and is a novel low-cost easily-operatable environment-friendly production method for biphenyltetracarboxylic dianhydride; moreover, isomeric compounds of all the biphenyltetracarboxylic dianhydride are synthesized at one time in the invention, so efficiency is improved and the cost is reduced.

Description

technical field [0001] The invention relates to the technical field of biphenyl dianhydride preparation, in particular to a method for preparing a biphenyl dianhydride mixture. Background technique [0002] Biphenyl dianhydride, also known as biphenyl tetra-acid dianhydride, has three isomers, namely 3,3'; 3,4; '-biphenyltetraic dianhydride, 2,3,2',3'-biphenyltetraic dianhydride and 2,3,3'4'-biphenyltetraic dianhydride. Biphenyl dianhydride is an important monomer for the synthesis of polyimide, a heat-resistant polymer material, and can be polymerized with various substances to prepare polyimide. Polyimide is currently an industrialized polymer material with superior comprehensive properties. It has been widely used in the fields of films, coatings, plastics, composite materials, adhesives, foam plastics, fibers, separation films, liquid crystal alignment agents and photoresists. Wide range of applications. Therefore, as an important monomer of high-performance polyimide...

Claims

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Application Information

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IPC IPC(8): C07D307/89
Inventor 魏东初李兵
Owner 苏州亚培克生物科技有限公司
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