Method for producing polyarylene sulfide, cyclic polyarylene sulfide pellet and method for producing same

A polyarylene sulfide and a technology for a manufacturing method are applied in the field of cyclic polyarylene sulfide particles and their manufacturing to achieve the effects of excellent transferability, molding processability, and low gas properties

Inactive Publication Date: 2014-11-05
TORAY IND INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the cyclic PAS obtained by this method is not disclosed at all about the problems during melt processing, that is, the amount of gas and the rate of weight loss, and there is no description at all

Method used

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  • Method for producing polyarylene sulfide, cyclic polyarylene sulfide pellet and method for producing same
  • Method for producing polyarylene sulfide, cyclic polyarylene sulfide pellet and method for producing same
  • Method for producing polyarylene sulfide, cyclic polyarylene sulfide pellet and method for producing same

Examples

Experimental program
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Embodiment

[0192] The present invention will be specifically described below with reference to examples. These examples are illustrative and not limiting.

[0193]

[0194] The molecular weights of PAS and cyclic PAS were calculated by gel permeation chromatography (GPC), which is one of size exclusion chromatography (SEC), in terms of polystyrene, and the number average molecular weight (Mn) and weight average molecular weight (Mw), and the molecular weight distribution was calculated by Mw / Mn calculation. The measurement conditions of GPC are shown below.

[0195] Device: Senshu Science SSC-7100

[0196] Column name: Showa Denko shodex UT806M

[0197] Eluent: 1-Chloronaphthalene

[0198] Detector: Differential Refractive Index Detector

[0199] Column temperature: 210°C

[0200] Pre-heating bath temperature: 250°C

[0201] Pump thermostat temperature: 50°C

[0202] Detector temperature: 210°C

[0203] Flow: 1.0mL / min

[0204] Sample injection volume: 300 µL (slurry state: a...

reference example 1

[0230] Add 1.648kg of 48% by weight aqueous solution of sodium hydrosulfide (sodium hydrosulfide 0.791kg (14.1 mole)), 1.225kg of 48% by weight aqueous solution of sodium hydroxide (sodium hydroxide 0.588 kg (14.7 moles)), N-methyl-2-pyrrolidone (NMP) 35 L, and p-dichlorobenzene (p-DCB) 2.278 kg (15.5 moles).

[0231] The reaction vessel was sealed under nitrogen at room temperature and normal pressure, and then the temperature was raised from room temperature to 200° C. over 25 minutes while stirring at 400 rpm. Next, it heated up to 250 degreeC over 35 minutes, and was made to react at 250 degreeC for 2 hours. Next, while maintaining the internal temperature at 250° C., the extraction valve was slowly opened, and 26.6 kg of the solvent was distilled off over 40 minutes. After the solvent was distilled off, the autoclave was cooled to around room temperature, and the contents were collected.

[0232] The recovered content was heated and stirred under nitrogen gas so that th...

reference example 2

[0234] Except having made the p-DCB of a raw material 2.116 kg (14.4 mol), and having made the solid-liquid separation temperature 50 degreeC, it carried out similarly to the reference example 1, and obtained the dry solid powder. From the analysis results of infrared absorption spectrum and high-performance liquid chromatography of the obtained dried solid, it was found that 85% by weight of cyclic polyphenylene sulfide was contained. The weight loss rate ΔWr(a) when heated at 200°C to 330°C was 1.439%.

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Abstract

By having a step (I) of heating under reduced pressure a cyclic polyarylene sulfide composition, and a step (II) of heating and polymerizing the same, the present invention is capable of achieving a high molecular weight form of polyarylene sulfide by a simple method and producing a polyarylene sulfide that has a small molecular weight distribution and has a low gassing tendency, thereby being industrially useful. Further, by pelletizing the composition after the step (I), cyclic polyarylene sulfide pellets can be produced which are excellent in transportability as well as moldability and processabilty, and which generate less gas and are therefore industrially useful.

Description

technical field [0001] The present invention relates to an industrially useful polyarylene sulfide comprising a step (I) of heating a cyclic polyarylene sulfide composition under reduced pressure and a step (II) of heating and polymerizing the cyclic polyarylene sulfide composition. Process for the manufacture of thioethers. In addition, it relates to an industrially useful cyclic polyarylene sulfide particle having excellent handleability and a small amount of gas generation, and a method for producing the same. Background technique [0002] Polyarylene sulfide represented by polyphenylene sulfide (hereinafter, polyarylene sulfide is sometimes abbreviated as PAS) is heat resistance, flame retardancy, chemical resistance, electrical insulation, heat and humidity resistance, mechanical strength and dimensional stability and other excellent engineering plastics. In addition, since PAS can be molded into various molded products, films, sheets, fibers, etc. by various molding ...

Claims

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Application Information

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IPC IPC(8): C08G75/06C08L81/02
CPCC08G75/06C08G75/02C08G75/14C08J2381/04B29B13/00C08J3/12
Inventor 鹿又昭纪西村阳介堀内俊辅海法秀竹田多完山内幸二铃木淳也
Owner TORAY IND INC
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