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Method for preparing 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 serious environmental pollution, long synthesis route, low total yield and the like

Active Publication Date: 2018-06-12
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

[0012] 32% by weight sodium hydroxide aqueous solution 79g (0.63mol) and 62.4g (0.3mol) bisphenol A were added to the reactor, stirred and heated up to dissolve, the temperature rose to 85℃, the solution was transparent, and then 510g trimethylbenzene solvent and 4.2g were added Benzyltriethylammonium chloride catalyst, heat and reflux for dehydration, the temperature rises to 172℃, the reaction is kept and stirred for 15 hours, then the temperature is reduced to 130℃, 108g (0.6mol) 4-chlorophthalic anhydride and 4.86g benzyltriethyl are added Base ammonium chloride catalyst, heated at 140℃~145℃, refluxed for 5 hours, then filtered while 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. The precipitate is filtered and washed with 250g of ethanol, stirred and refluxed for 2 hours, filtered, and 125g of wet material is obtained. After drying, 120g of...

Embodiment 2

[0014] 55.2g (0.69mol) of 50% by weight sodium hydroxide aqueous solution and 62.4g (0.3mol) of bisphenol A were added to the reactor, stirred and heated up to dissolve, the temperature rose to 85℃, the solution was transparent, and then 510g of trimethylbenzene solvent and 4.2 g benzyltriethylammonium chloride catalyst, heated and refluxed for dehydration, the temperature was increased to 172℃, and the reaction was kept stirring for 18 hours, then the temperature was reduced to 130℃, 114g (0.63mol) 4-chlorophthalic anhydride and 4.86g benzyltri Ethylammonium chloride catalyst, heated at 140℃~145℃, refluxed for 5 hours, then filtered while 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 After filtering, the precipitate is washed with 250g ethanol, stirred and refluxed for 2 hours, filtered, and 118g of wet material is obtained. After drying, 113g ...

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Abstract

The invention relates to a method for preparing bisphenol A diether dianhydride. The method comprises the following steps that: the molar ratio of sodium hydroxide to bisphenol A is (2.1-2.3) to 1, the molar ratio of 4-chlorophthalic anhydride to phenol A is (2-2.1) to 1, the weight of a catalyst benzyl triethyl ammonium chloride is 15% by weight of the weight of bisphenol A, and the amount of a solvent trimethylbenzene is 8 times larger than the weight of bisphenol A; the preparation process is as follows: adding an aqueous solution of sodium hydroxide and bisphenol A to areactor, heating, stirring and dissolving at a temperature, heating to 85 DEG C to 90 DEG C, adding the trimethylbenzene and benzyl triethyl ammonium chloride which accounts 46% by weight of the total weight, heating toreflux, dewatering, stirring at a temperature of 172 DEG C and reacting for 15 to 18 hours, cooling to 130 DEG C, adding 4-chlorophthalic anhydride and benzyl triethyl ammonium chloride which accounts54% by weight of the total weight, heating 140 DEG C to 145 DEG C, performing a reflux reaction for 5 to 6 hours, filtering while hot, cooling a filtrate to room temperature, filtering, washing a precipitate with deionized water and ethanol respectively, filtering to obtain a wet material, and drying to obtain a bisphenol A diether dianhydride product with a yield of 80 to 85%. .

Description

1. Technical Field [0001] The present invention relates to a method for preparing bisphenol A diether dianhydride, and more specifically to a method for preparing bisphenol A diether dianhydride for preparing polyetherimide. 2. Background technology [0002] 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. Its dosage accounts for more than 50% of the total polyimide dosage. Polyetherimide has the following characteristic properties: high strength and high hardness at room temperature and high temperature, long-term temperature resistance, highly stable size and electrical properties, wide range of chemical resistance, thermoplastic processing methods and molding equipment for melt processing, Mass production, inherent flame retardancy, low smoke during combustion. It is widely used in high temperature tech...

Claims

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Application Information

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Patent Type & Authority Applications(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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