Method for producing bisphthalonitrile terminated diphenyl sulfide oligomer

A bis-phthalonitrile and diphenylene sulfide technology, applied in the direction of sulfide preparation, organic chemistry, etc., can solve the problems of outdated methods, high energy consumption, cumbersome processes, etc., achieve simple methods, overcome pollution, and reduce production cost effect

Inactive Publication Date: 2011-06-08
自贡鸿鹤化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the above-mentioned background technology has defects such as outdated method for recovering phenylene sulfide oligomers, cumbersome process, high energy consumption, and failure to effectively utilize the recovered PPS resin in the recovered phenylene sulfide oligomers and by-products.

Method used

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Examples

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Embodiment

[0022] A. Take 100g of the slurry (waste residue) formed during the production process of polyphenylene sulfide and the product purification process, add 150ml of clean water each time and wash 3 times continuously to remove salt, residual solvent and water-soluble impurities; remove the impurities The density of the material is 1.30g / cm 3 Then, add diluted hydrochloric acid with a concentration of 1.0 wt% under stirring conditions, and acidify the slurry until the pH of the slurry is 7-9; filter the acidified slurry to obtain phenylsulfide oligomerization The solid mixture of material and polyphenylene sulfide, ready for use after drying;

[0023] B. Massage the sulphur source Na 2 S 5g, sodium hydroxide 2.5g, 60ml N-methyl-2-pyrrolidone (NMP), added to the reactor, replaced the air with nitrogen, then heated to 220 ℃ to remove water for 1 hour, the system was cooled to 90 ℃, add 6.3 g of polyphenylene sulfide and polyphenylene sulfide oligomer obtained in step A were reacted at...

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Abstract

The invention relates to a method for producing bisphthalonitrile terminated diphenyl sulfide oligomer, belonging to the field of high molecular synthetic materials. The method comprises the following steps: separating and purifying slurry generated in the processes of ployphenylene sulfite (PPS) resin production and product purification so as to recover a mixture of polyphenylene sulfide oligomer and residual PPS resin; carrying out cracking and thiol-termination on the mixture to obtain dithiol-terminated polyphenylene sulfide oligomer; and synthesizing the dithiol-terminated polyphenylene sulfide oligomer with 4-nitrophthalonitrile, so as to obtain the bisphthalonitrile terminated diphenyl sulfide oligomer. In the invention, the method is simple, the yield is high, and the useful byproducts in the discharged slurry (waste slag) can be fully utilized, thereby effectively overcoming the pollution of the waste slag on environment and restriction of the waste slag on production scale and reducing the production cost of enterprises; and the prepared bisphthalonitrile terminated diphenyl sulfide oligomer can be used for producing phthalonitrile with a phthalocyanine ring structure and the like.

Description

Technical field [0001] The invention belongs to a method for producing bisphthalonitrile-terminated phenylsulfide oligomers in the field of polymer synthetic materials, and particularly relates to a by-product and 4-nitrophthalene sulfide produced in the production process of polyphenylene sulfide. A method for producing bis-phthalonitrile end-group phenyl sulfide oligomer with dimethyl cyanide as a raw material. Background technique [0002] In the production process of polyphenylene sulfide (PPS), a slurry containing 6-8wt% phenylene sulfide oligomer and 0.5wt% of residual PPS resin by-products will be produced after solvent recovery. The amount of slurry generally accounts for 12-15 wt% of the input amount of production raw materials. For the treatment of these by-products, the conventional method is to first concentrate them into ore mud, and then directly incinerate or discard them as waste; the former requires high energy consumption and will also cause air pollution, whil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/62C07C319/14
Inventor 高健唐国强冉蓉王晓龙林雪梅廖斌
Owner 自贡鸿鹤化工股份有限公司
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