Process for synthesizing low-chlorine film polyphenylene sulfide resin

A technology of polyphenylene sulfide resin and synthesis process, which is applied in the field of polymer material resin synthesis, can solve problems such as unseen process introduction, and achieve the effects of improving production efficiency, increasing reaction speed, and saving costs

Active Publication Date: 2011-07-27
SICHUAN DEYANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 sodium bicarbonate and Sodium hydrosulfide specific process introduction

Method used

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

Examples

Experimental program
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Embodiment 1

[0024] In a 1L dehydration kettle, add sodium sulfide (Na 2 S.5H 2 O) 2.0mol, under the protection of 99.99% nitrogen, heat the temperature to 120°C, and then vacuumize and dehydrate under the condition of maintaining the temperature and pressure at -0.3Mpa, so that the moles of sodium sulfide and water in the sodium sulfide solution The ratio becomes 1:1.2, then use the 4.5mol / molNa 2 The NMP solvent of S is added from the top of the dehydration column of the molecular sieve, directly flows into the 2L high-pressure reactor, and then NaOH is added to the reactor with a molar mass of 0.1mol / molNa 2 S, after raising the temperature to 130°C, add 2mol of p-dichlorobenzene. Then replace the air in the reactor with nitrogen 3-5 times, then seal the reactor, the temperature rises to 238°C, and keeps at this temperature for 2h, and when the temperature drops to 130°C, add 0.1mol / molNa 2 For the industrial grade sodium bicarbonate of S, the temperature rises to 238°C and is kept a...

Embodiment 2

[0026] In a 1L dehydration kettle, add sodium sulfide (Na 2 S.5H 2 O) 2.0mol, under the protection of 99.99% nitrogen, heat the temperature to 125°C, and then vacuumize and dehydrate under the condition of maintaining the temperature and pressure at -0.3Mpa, so that the moles of sodium sulfide and water in the sodium sulfide solution The ratio becomes 1:1.3, then use the 4.5mol / molNa 2 The NMP solvent of S is added from the top of the dehydration column of the molecular sieve, directly flows into the 2L high-pressure reactor, and then NaOH is added to the reactor with a molar mass of 0.2mol / molNa 2 S, after raising the temperature to 135°C, add 2 mol of p-dichlorobenzene. Then replace the air in the reactor with nitrogen 3-5 times, and then seal the reactor, the temperature rises to 240°C, and keeps at this temperature for 2.5h, and when the temperature drops to 135°C, add 0.04mol / molNa 2 For industrial grade sodium bicarbonate of S, the temperature rises to 240°C and is ke...

Embodiment 3

[0028] In a 1L dehydration kettle, add sodium sulfide (Na 2 S.5H 2 O) 2.0mol, under the protection of 99.99% nitrogen, heat the temperature to 130°C, and then vacuumize and dehydrate under the condition of maintaining the temperature and pressure at -0.3Mpa to make the molar ratio of sodium sulfide and 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 dehydration column of the molecular sieve, directly flows into the 2L high-pressure reactor, and then NaOH is added to the reactor with a molar mass of 0.3mol / molNa 2 S, after raising the temperature to 140°C, add 2mol of p-dichlorobenzene. Then replace the air in the reactor with nitrogen 3-5 times, then seal the reactor, the temperature rises to 242°C, and keeps at this temperature for 3h, and when the temperature drops to 140°C, add 0.05mol / molNa 2 For industrial grade sodium bicarbonate of S, the temperature rises to 242°C, and after keeping at th...

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Abstract

The invention discloses a process for synthesizing a low-chlorine film polyphenylene sulfide resin. In the process, sodium sulfide and santochlor are taken as raw materials, N-methyl-2pyrrolidone (NMP) is used as a solvent, and the ratio of sodium sulfide to santochlor to NMP to NaOH to sodium bicarbonate to NaHS is 1:1:3.9:(0.2-0.3):(0.2-0.3):0.05. The process comprises the following steps: in the dehydration period of the sodium sulfide, under the condition of relative low temperature of 120-130 DEG C and pressure of -0.3MPa and the protection of nitrogen, carrying out vacuum dehydration on the sodium sulfide to obtain the sodium sulfide solution of which the moisture content is 1.0-1.2mol/mol Na2S; adding NaOH, NMP and P-DCB at a corresponding molar ratio; and finally reducing the temperature at a temperature-reducing speed of 30 DEG C/min, and washing and drying to obtain the low-chlorine film polyphenylene sulfide resin required in the invention. The product in the invention has low total content of Halogens, low volatile matter and polydispersity index, narrow molecular weight distribution, high oxygen index, and excellent dielectric properties, and can be used as an insulating material or packaging material for electronic and electrical equipment.

Description

technical field [0001] The invention belongs to the synthesis of polymer material resin, especially the field of polyphenylene sulfide resin production. Background technique [0002] High-performance polyphenylene sulfide has excellent chemical resistance and thermal stability at high temperatures, and has flame retardancy, insulation, radiation resistance and good mechanical properties. In order to explore the synthesis method of this material, researchers from all over the world have been working hard to find it. [0003] In U.S. Patent No: 4761468, it is described to use chemical substances such as mercapto and mercapto metal salts to treat the polyphenylene sulfide resin after the polyphenylene sulfide resin is synthesized, thereby reducing the content of chlorine in the polyphenylene sulfide resin. Later, polyphenylene sulfide resin is applied to the field of electronic components through modification, and its main purpose is to improve the insulation performance of po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G75/0254
Inventor 苟梁武刘彬单彤包兴泽刘文良刘鑫胡良王益茂曹华徐伟蒋每雄
Owner SICHUAN DEYANG CHEM
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