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A kind of preparation method of bisphenol A diether dianhydride

A technology of diether dianhydride and bisphenol is applied in the field of preparation of bisphenol A diether dianhydride, and can solve the problems of long synthesis route, low total yield, and generation of a large amount of waste acid.

Active Publication Date: 2021-06-08
上海固创化工新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis route of this method is long, the total yield is low, and a large amount of waste acid and waste alkali are produced in the production process, which seriously pollutes the environment. It is really necessary to improve the production method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 79g (0.63mol) and 62.4g (0.3mol) of 32% by weight sodium hydroxide aqueous solution into the reactor, stir and heat up to dissolve, the temperature rises to 85°C and the solution is transparent, then add 510g trimethylbenzene solvent and 4.2g Benzyltriethylammonium chloride catalyst, heat up and reflux for dehydration, the temperature rises to 172°C, heat and stir for 15 hours, then cool down to 130°C, add 108g (0.6mol) 4-chlorophthalic anhydride and 4.86g benzyltriethyl ammonium chloride catalyst, raised the temperature to 140°C to 145°C, refluxed for 5 hours, then filtered while it was hot, pumped the filtrate into a crystallization kettle, cooled the filtrate to room temperature, crystallized for 12 hours, filtered, and washed the precipitate with deionized water. Filter to obtain the precipitate and wash it with 250g of ethanol, stir and reflux for 2 hours, filter to obtain 125g of wet material, and dry to obtain 120g of bisphenol A diether dianhydride product (y...

Embodiment 2

[0018] 55.2g (0.69mol) of 50% by weight aqueous sodium hydroxide solution and 62.4g (0.3mol) bisphenol A are added in the reactor, stirred and heated up to dissolve, the temperature rises to 85 ℃ and the solution is transparent, then add 510g trimethylbenzene solvent and 4.2 g benzyltriethylammonium chloride catalyst, heat up to reflux for dehydration, raise the temperature to 172°C, keep stirring for 18 hours, then cool down to 130°C, add 114g (0.63mol) of 4-chlorophthalic anhydride and 4.86g of benzyltri Ethyl ammonium chloride catalyst, heat up to 140°C to 145°C, reflux for 5 hours, then filter while hot, pump the filtrate into a crystallization kettle, cool the filtrate to room temperature, crystallize for 12 hours, filter, and wash the precipitate with deionized water , filtered, and the precipitate was washed with 250g ethanol, stirred and refluxed for 2 hours, filtered to obtain 118g of wet material, and after drying, 113g (yield 80%) of bisphenol A diether dianhydride p...

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Abstract

The present invention relates to a kind of preparation method of bisphenol A diether dianhydride, and the method comprises the following steps; The ratio is 2 to 2.1:1, the weight of the catalyst benzyltriethylammonium chloride is 15% by weight of the weight of bisphenol A, and the amount of the solvent trimethylbenzene is 8 times of the weight of bisphenol A; the preparation process is: sodium hydroxide Add the aqueous solution and bisphenol A into the reactor, raise the temperature and stir to dissolve, raise the temperature to 85°C-90°C, add trimethylbenzene and benzyltriethylammonium chloride accounting for 46% by weight of the total, heat up to reflux, dehydrate, and stir at 172°C React for 15-18 hours, lower the temperature to 130°C, add 4-chlorophthalic anhydride and benzyltriethylammonium chloride accounting for 54% by weight of the total, raise the temperature to 140°C-145°C, reflux for 5-6 hours, and Filtrate, cool the filtrate to room temperature, filter, wash the precipitate with deionized water and ethanol respectively, and filter to obtain a wet material, dry to obtain a bisphenol A diether dianhydride product with a yield of 80-85%.

Description

[0001] 1. Technical field [0002] The invention relates to a preparation method of bisphenol A diether dianhydride, more specifically to a preparation method of bisphenol A diether dianhydride used for preparing polyetherimide. [0003] 2. Background technology [0004] Polyetherimide is prepared by reacting bisphenol A diether dianhydride with 4.4'-diaminodiphenyl ether or 4.4'-diaminodiphenylmethane or m-phenylenediamine. Polyetherimide is a thermoplastic resin with a wide range of uses, and its consumption accounts for more than 50% of the total polyimide consumption. Polyetherimide has the following characteristic properties: high strength and high hardness at room temperature and high temperature, long-term temperature resistance, high stability in size and electrical properties, wide range of chemical resistance, melt processing using thermoplastic processing methods and molding equipment, Mass produced, inherently flame retardant and low smoke when burned. Widely used...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/89
CPCC07D307/89
Inventor 刘少华
Owner 上海固创化工新材料有限公司
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