Preparation method of 3,3',4,4'-diphenyl sulfone tetracarboxylicdianhydride

A technology of diphenyl sulfone tetracarboxylic dianhydride and diphenyl sulfide tetracarboxylic dianhydride, which is applied in the preparation of monomer 3,3′,4,4′-diphenylsulfone tetracarboxylic dianhydride It can solve problems such as high requirements for reaction equipment, difficulty in purchasing catalysts, and increased production costs.

Active Publication Date: 2017-03-22
天津众泰材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The catalyst used in the above two methods is special and difficult to purchase, and the catalyst has a large molecular weight and is not easy to recycle, resulting in increased prod

Method used

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  • Preparation method of 3,3',4,4'-diphenyl sulfone tetracarboxylicdianhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 18.2g of 4-chlorophthalic anhydride, 120g of dimethyl sulfoxide, 0.77g of sulfur and 14.4g of sodium tert-butoxide to the reaction kettle, then raise the temperature to 40°C and drop in 11g of carbon disulfide (the molar ratio is: 4-chlorophthalic anhydride: carbon disulfide: Sulfur: sodium tert-butoxide: dimethyl sulfoxide = 1: 1.4: 0.03: 1.5: 15), after the dropwise addition is completed, the temperature is raised to 150 ° C to react until the raw materials are completely reacted, and part of the dimethyl sulfoxide is recovered under reduced pressure, and the remaining Add water, filter, wash with water, and dry to obtain 32.2 g of 3,3',4,4'-diphenylsulfide tetracarboxylic dianhydride, with a yield of 98.77%.

[0030] Add 16.3g 3,3',4,4'-diphenylsulfide tetracarboxylic acid diacid, 320g acetonitrile, 1.9g cerium ammonium nitrate, 0.9g tetrabutylammonium iodide and 160g water in the reaction kettle, heat up Add 16.2g potassium persulfate in batches to 40°C (molar r...

Embodiment 2

[0032] Add 18.2g of 4-chlorophthalic anhydride, 78g of dimethyl sulfoxide, 0.26g of sulfur and 11.5g of sodium tert-butoxide in the reactor, then add 8.4g of carbon disulfide dropwise to 40°C (the molar ratio is: 4-chlorophthalic anhydride: carbon disulfide : sulfur: sodium tert-butoxide: dimethyl sulfoxide = 1: 1.1: 0.01: 1.2: 10), after the dropwise addition is completed, the temperature is raised to 120 ° C to react until the raw materials are completely reacted, and part of the dimethyl sulfoxide is recovered under reduced pressure, and the remaining The mixture was added into water, filtered, washed with water, and dried to obtain 27.3g of 3,3',4,4'-diphenylsulfide tetracarboxylic dianhydride, with a yield of 83.74%.

[0033] In reactor, add 16.3g3,3',4,4'-diphenylsulfide tetracarboxylic acid diacid, 260g acetonitrile, 1.4g cerium ammonium nitrate, 0.2g tetrabutylammonium iodide and 130g water, be warmed up to Add 13.5g potassium persulfate in batches at 20°C (molar ratio...

Embodiment 3

[0035] Add 18.2g of 4-chlorophthalic anhydride, 156g of dimethyl sulfoxide, 1.3g of sulfur and 17.3g of sodium tert-butoxide to the reaction kettle, then raise the temperature to 40°C and drop in 13g of carbon disulfide (the molar ratio is: 4-chlorophthalic anhydride: carbon disulfide: Sulfur: sodium tert-butoxide: dimethyl sulfoxide = 1: 1.7: 0.05: 1.8: 20), after the dropwise addition is completed, the temperature is raised to 150 ° C to react until the raw materials are completely reacted, and part of the dimethyl sulfoxide is recovered under reduced pressure, and the remaining Add water, filter, wash with water, and dry to obtain 32.3 g of 3,3',4,4'-diphenylsulfide tetracarboxylic dianhydride, with a yield of 99.08%.

[0036]In reactor, add 16.3g3,3',4,4'-diphenylsulfide tetracarboxylic acid diacid, 400g acetonitrile, 2.7g ammonium cerium nitrate, 1.8g tetrabutylammonium iodide and 200g water, heat up to Add 16.2g potassium persulfate in batches at 60°C (molar ratio: 3,3′,...

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Abstract

The invention discloses a preparation method of 3,3',4,4'-diphenyl sulfone tetracarboxylicdianhydride. The preparation method comprises the following steps that 1, 4-chlorophthalic anhydride is dissolved into dimethyl sulfoxide, then sulfur and sodium tert-butoxide are added, carbon disulfide is dropwise added when the temperature is increased to 40 DEG C, after the raw materials completely react, part of the solvent is recycled under reduced pressure, a remaining product is added into water, and filtering, water washing and drying are conducted to obtain 3,3',4,4'-diphenyl thioether tetracarboxylicdianhydride; 2, 3,3',4,4'-diphenyl thioether tetracarboxylicdianhydride is dissolved into acetonitrile, ceric ammonium nitrate, tetrabutylammonium iodide and water are added, potassium persulfate is added in batches under the heating condition, after 3,3',4,4'-diphenyl thioether tetracarboxylicdianhydride completely reacts, water is added into reaction liquid, the temperature is lowered to 5 DEG C, filtering, water washing and drying are conducted, and 3,3',4,4'-diphenyl sulfone tetracarboxylicdianhydride is obtained. The preparation method of 3,3',4,4'-diphenyl sulfone tetracarboxylicdianhydride has the following advantages that the raw materials are easy to purchase, the reaction solvent can be recycled, aftertreatment operation is easy, the yield is high, the product quality is good, and environmental pollution is low.

Description

technical field [0001] The invention relates to a preparation method of a monomer 3,3',4,4'-diphenylsulfone tetracarboxylic dianhydride which can be used as a polyimide monomer material. Background technique [0002] 3,3′,4,4′-Diphenylsulfonetetracarboxylic dianhydride is an aromatic polyimide monomer material, because of its heat resistance, chemical resistance plus excellent mechanical strength and Electrical properties, widely used as high-performance components of electronic products, various industrial machinery, automobiles, aircrafts, etc. [0003] The preparation method of 3,3',4,4'-diphenylsulfone tetracarboxylic dianhydride is reported as follows: [0004] 1) Sakakura, Akira et al. provided a method for preparing 3,3′,4,4′-diphenylsulfone tetracarboxylic dianhydride by dehydration: using 3,3′,4,4′-tetracarboxylic diphenylsulfone A special boric acid catalyst was used as the raw material to heat and dehydrate at 115°C for 12 hours to obtain 3,3′,4,4′-diphenylsulfo...

Claims

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Application Information

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IPC IPC(8): C07D307/89
CPCC07D307/89
Inventor 尚振华栗晓东张鹏飞刘金燕
Owner 天津众泰材料科技有限公司
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