Preparation method of polyarylene sulfide film

A polyarylene sulfide and film technology, which is applied in the field of polyarylene sulfide film preparation, can solve the problems of inability to prepare high-toughness films, high resin crystallinity, and many reaction by-products, etc., and achieves easy processing and high molecular weight. , the effect of low cost

Active Publication Date: 2011-07-20
SICHUAN UNIV
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Problems solved by technology

Such as Philips company prepares (US 33544129) with sodium sulfide and p-dichlorobenzene in nitrogen in the polar solvent NMP pressurized reaction, this method energy consumption is big, and cost is high
Chinese patent CN1143652A reports that in a polar solvent, sulfur is used as a raw material to pressurize and synthesize tough polyphenylene sulfide resin. The reaction process requires the use of a reducing agent, the process is relatively complicated, there are many reaction by-products, and the product is not easy to purify; CN1793202A Deyang Technology Co., Ltd. Co., Ltd. uses sodium sulfide and p-dichlorobenzene as raw materials to pressurize synthetic fiber-grade polyphenylene sulfide resin with a catalytic system, but the resulting resin has high crystallinity and cannot be used to prepare high-toughness films

Method used

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  • Preparation method of polyarylene sulfide film
  • Preparation method of polyarylene sulfide film
  • Preparation method of polyarylene sulfide film

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Add 100g of sodium benzoate, 80g of p-aminotoluene, 20g of sodium hydroxide and 600g of dimethylacetamide into a reaction kettle equipped with a nitrogen inlet and outlet, a water separator, a stirrer and a thermometer. After stirring evenly, add 60% 130g of sodium sulfide was dehydrated at a temperature of 160°C for 3 hours under the protection of nitrogen to obtain dehydrated Na 2 S solution, to be the above Na 2 When the temperature of the S solution drops to 80°C, add 117.6g of p-dichlorobenzene and 43.6g of 4,4'-difluorobenzophenone, react at a temperature of 180°C for 8 hours, and then keep it at 250°C for 8 hours. The liquid was hot filtered to separate the solvent and the polymer. After the polymer was washed and dried, it was purified with deionized water and acetone, and dried at a temperature of 120°C and a vacuum of 0.09 MPa for 24 hours to obtain a film-grade polyarylene sulfide resin. The yield was 87%, and the intrinsic viscosity η=0.22.

[0035] The ab...

Embodiment 2

[0037] Add 5g of trisodium phosphate, 20g of sodium p-aminobenzenesulfonate, 100g of sodium bicarbonate and 200g of hexamethylphosphoric triamide into a reaction kettle with a nitrogen inlet and outlet, a water separator, a stirrer and a thermometer, and stir evenly , adding 130 g of sodium sulfide with a content of 60%, under the protection of nitrogen, dehydration reaction at a temperature of 200 ° C for 3 hours, to obtain Na after dehydration 2 S solution, to be the above Na 2 When the temperature of the S solution drops to 150°C, add 132.3g p-dichlorobenzene and 14.7g m-dichlorobenzene, react at a temperature of 250°C for 1 hour, then keep at 300°C for 3 hours, heat filter the reaction solution, and separate the solvent And the polymer, the polymer is washed and dried, then purified with deionized water and acetone, and dried at a temperature of 120° C. under a vacuum of 0.09 MPa for 24 hours to obtain a film-grade polyarylene sulfide resin. The yield is 85%, and the intr...

Embodiment 3

[0040] Add 10g of lithium chloride, 20g of ε-aminocaproic acid, 10g of potassium carbonate and 500g of sulfolane into a reaction kettle with a nitrogen inlet and outlet, a water separator, a stirrer and a thermometer, and after stirring evenly, add sulfide with a content of 60%. Sodium 130g, under the protection of nitrogen, dehydration reaction at a temperature of 180 ° C for 0.5 hours to obtain the dehydrated Na 2 S solution, to be the above Na 2 When the temperature of the S solution drops to 110°C, add 132.3g of p-dichlorobenzene and 28.7g of 4,4'-dichlorodiphenyl sulfone, react at a temperature of 180°C for 3 hours, and then keep it at 280°C for 4 hours. Heat filtration to separate the solvent and the polymer. After the polymer is washed and dried, it is purified with deionized water and acetone, and dried at a temperature of 120°C and a vacuum of 0.09 MPa for 24 hours to obtain a film-grade polyarylene sulfide resin. The yield is 89%, and the intrinsic viscosity η=0.29....

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Abstract

The invention discloses a preparation method of polyarylene sulfide film, characterized by comprising the following steps of: adding 5-100 parts of auxiliaries, 20-80 parts of catalyst, 1-100 parts of alkali and 200-600 parts of organic solvent to a reaction kettle with a nitrogen inlet/outlet pipe, a water separator, a stirrer and a thermometer; adding 130 parts of 60% sodium sulfide, under nitrogen protection, performing dehydration reaction at the temperature of 160-200 DEG C for 0.5-3 hours; cooling to 80-150 DEG C, adding 147-352 parts of aromatic compound polyhalide, reacting at the temperature of 110-250 DEG C for 1-8 hours; keeping at the temperature of 160-320 DEG C for 1-8 hours; filtering the reactant liquor, separating, washing the polymer, drying, purifying with deionized water and acetone, and drying at the temperature of 120 DEG C and the vacuum degree of 0.09MPa for 24 hours to obtain the high molecular weight polyarylene sulfide film-grade resin; preparing the high molecular weight polyarylene sulfide film-grade resin into polyarylene sulfide resin particles by twin screw extrusion granulation; drying the polyarylene sulfide resin particles at the temperature of 100-120 DEG C for 4-10 hours and extruding to form film of 1-3mm in a casting machine; and laterally stretching the film for 2-10 times and then longitudinally stretching the film for 2-10 times in a two-way film stretching machine to prepare the film with even thickness.

Description

technical field [0001] The invention relates to a preparation method of a polyarylene sulfide film, which belongs to the field of polymer synthesis. Background technique [0002] Polyarylene sulfide, such as polyphenylene sulfide, polyphenylene sulfide ketone, and polyphenylene sulfide sulfone, can be widely used in automobiles, aerospace and aviation due to its high temperature resistance, corrosion resistance, excellent electrical properties, mechanical properties and dimensional stability , electronics and food engineering technology. In industrial production, polyarylene sulfide is mainly prepared by sodium sulfide or sulfur solution method. Such as Philips company prepares (US 33544129) with sodium sulfide and p-dichlorobenzene pressurized reaction in the polar solvent NMP in nitrogen, this method energy consumption is big, and cost is high. Chinese patent CN1143652A reports that in a polar solvent, sulfur is used as a raw material to pressurize and synthesize tough p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08L81/02B29C55/14B29C41/52C08G75/0213C08G75/0236C08G75/024C08G75/0254
Inventor 杨杰张刚黄宝奎龙盛如王孝军
Owner SICHUAN UNIV
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