Process for synthesizing low-chlorine polyphenylene sulfide resin

A polyphenylene sulfide resin and a synthesis process technology are applied in the field of polymer material resin synthesis to achieve the effects of improving reaction speed, saving costs and shortening synthesis time.

Active Publication Date: 2012-01-11
四川得阳特种新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] As far as the existing polyphenylene sulfide synthesis technology is concerned, the synthesis of polyphenylene sulfide resin generally uses sodium sulfide and p-dichlorobenzene (P-DCB) as raw materials, although the American Phillips company and Japanese polyphenylene sulfide resin The polyphenylene sulfide resin produced by the production company has basically not changed much in raw materials, so that the polyphenylene sulfide resin can achieve the purpose of low chlorine by adding auxiliary materials, but it has not been mixed with other Na 2 SO 4 and hydrogen sulfide specific process introduction

Method used

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  • Process for synthesizing low-chlorine polyphenylene sulfide resin
  • Process for synthesizing low-chlorine polyphenylene sulfide resin

Examples

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Effect test

Embodiment 1

[0024] In a 1L dehydration kettle, add sodium sulfide (Na 2 S.5H 2 O) 2.0mol, at 99.99% CO 2 Under the protection of gas, the temperature is heated to 120℃, and the input holding temperature is 120℃. Equipped with three layers of 18cm / layer 5 angstrom molecular sieve water absorption column. After the molecular sieve absorbs water, the molar ratio of sodium sulfide to water in the sodium sulfide solution becomes 1:1.2, then use 4.5mol / molNa 2 The NMP solvent of S is added from the top of the water absorption column of the molecular sieve, and directly flows into the 2L autoclave, and then the molar mass of NaOH is 0.1mol / molNa in the reactor. 2 S, after raising the temperature to 130°C, add 2 mol of p-dichlorobenzene. Replace the air in the reactor with carbon dioxide gas 3-5 times, and then seal the reactor. After the reactor is sealed, the temperature rises to 238℃, and keeps it at this temperature for 2h, and when the temperature drops to 130℃, add 0.1mol / molNa 2 S's industria...

Embodiment 2

[0026] In a 1L dehydration kettle, add sodium sulfide (Na 2 S.5H 2 O) 2.0mol, at 99.99% CO 2 Under the protection of gas, the temperature is heated to 125℃, and the input holding temperature is 125℃. Equipped with three layers of 18cm / layer 5 angstrom molecular sieve water absorption column. After the molecular sieve absorbs water, the molar ratio of sodium sulfide to water in the sodium sulfide solution becomes 1:1.3, then use 4.5mol / molNa 2 The NMP solvent of S is added from the top of the water absorption column of the molecular sieve, and directly flows into the 2L autoclave, and then the molar mass of NaOH is 0.2mol / molNa in the reactor. 2 S, after raising the temperature to 135°C, add 2 mol of p-dichlorobenzene. Replace the air in the reactor with carbon dioxide gas 3-5 times, and then seal the reactor. After the reactor is closed, the temperature rises to 240℃, and keeps it at this temperature for 2.5h, and when the temperature drops to 135℃, add 0.04mol / molNa 2 S's indust...

Embodiment 3

[0028] In a 1L dehydration kettle, add sodium sulfide (Na 2 S.5H 2 O) 2.0mol, at 99.99% CO 2 Under the protection of gas, the temperature is heated to 130℃, and the input holding temperature is 130℃. Equipped with three layers of 18cm / layer 5 angstrom molecular sieve water absorption column. After the molecular sieve absorbs water, the molar ratio of sodium sulfide to water in the sodium sulfide solution becomes 1:1.5, then use 4.5mol / molNa 2 The NMP solvent of S is added from the top of the water absorption column of the molecular sieve, and directly flows into the 2L autoclave, and then the molar mass of NaOH is 0.3mol / molNa in the reactor. 2 S, after raising the temperature to 140°C, add 2 mol of p-dichlorobenzene. Replace the air in the reactor with carbon dioxide gas 3-5 times, and then seal the reactor. After the reactor is sealed, the temperature rises to 242℃, and keeps it at this temperature for 3h, and when the temperature drops to 140℃, add 0.05mol / molNa 2 S's industri...

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Abstract

The invention discloses a process for synthesizing low-chlorine polyphenylene sulfide resin. Sodium sulfide and paradichlorobenzene are used as raw materials, N-methyl-2-pyrrolidone is used as a solvent, and the molar ratio of the sodium sulfide to the paradichlorobenzene is 1:1. The synthesis process mainly comprises the following steps of: in a sodium sulfide dehydration treatment phase, carrying out sodium sulfide solution insulating and water sucking treatment by adopting three layers of 18cm water sucking column containing a 5 angstrom molecular sieve in each layer to form a sodium sulfide solution with the water content of 1.2-1.5mol / molNa2S and adding NaOH with the molar mass of 0.1-0.3mol / molNa2S; and in the polycondensation phase, adding Na2SO4 of 0.1-0.05mol / molNa2S and H2S gas of 0.01mol / molNa2S. The invention has lower halogen total content and polydispersion coefficient in the obtained product, narrow molecular weight distribution, high oxygen index and excellent electrical insulating property and can be used as a packaging material of an electronic device.

Description

Technical field [0001] The invention belongs to the field of polymer material resin synthesis, especially polyphenylene sulfide resin production. Background technique [0002] High-performance polyphenylene sulfide has excellent chemical resistance and thermal stability at high temperatures, and has flame retardant, insulation, radiation resistance and good mechanical properties. In order to explore the synthesis method of this material, researchers from various countries have been constantly seeking for it. [0003] U.S. Patent No: 4761468 describes the use of chemical substances such as mercapto and mercapto metal salts to treat polyphenylene sulfide resin after synthesis of polyphenylene sulfide resin, thereby reducing the content of chlorine in polyphenylene sulfide resin. Later, polyphenylene sulfide resin was applied to the field of electronic components through modification, and its main purpose was to improve the insulation performance of polyphenylene sulfide materials. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/02C08G75/0213C08G75/0254
Inventor 苟梁武胥德强刘彬包兴泽李贤虎杨华龚海明刘文良徐伟蒋每雄
Owner 四川得阳特种新材料有限公司
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