Polyarylene sulfide production method and polyarylene sulfide

A technology of polyarylene sulfide and its manufacturing method, which is applied in the field of polyarylene sulfide manufacturing, can solve the problems of increased cost of polyarylene sulfide, and achieve the effect of low gas and high molecular weight

Inactive Publication Date: 2013-06-26
TORAY IND INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In general, cyclic oligomers are obtained as a mixture with a large amount of linear oligomers, so in order to obtain high-purity cyclic oligomers, a high

Method used

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  • Polyarylene sulfide production method and polyarylene sulfide
  • Polyarylene sulfide production method and polyarylene sulfide
  • Polyarylene sulfide production method and polyarylene sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0122] The present invention will be specifically described below with reference to examples. These examples are illustrative and not limiting.

[0123]

[0124] The molecular weights of polyarylene sulfide and cyclic polyarylene sulfide were calculated in terms of polystyrene by number average molecular weight (Mn) and weight average molecular weight by gel permeation chromatography (GPC), which is one of size exclusion chromatography (SEC). Molecular weight (Mw). The measurement conditions of GPC are shown below.

[0125] Device: Senshu Science SSC-7100

[0126] Column name: センシューscience GPC3506

[0127] Eluent: 1-Chloronaphthalene

[0128] Detector: Differential Refractive Index Detector

[0129] Column temperature: 210°C

[0130] Pre-heating bath temperature: 250°C

[0131] Pump thermostat temperature: 50°C

[0132] Detector temperature: 210°C

[0133] Flow: 1.0mL / min

[0134] Sample injection volume: 300 μL (slurry form: about 0.2% by weight).

[0135]

[0...

reference example 1

[0188] Reference Example 1 (Preparation of Cyclic Polyarylene Sulfide Composition)

[0189] A stainless steel autoclave equipped with a stirrer was used as a reaction vessel. In the reaction container, 14.03 g (0.120 mol) of a 48% by weight aqueous solution of sodium hydrosulfide, 12.50 g (0.144 mol) of a 48% by weight aqueous solution of sodium hydroxide prepared using 96% sodium hydroxide, and N-methyl-2 - 615.0 g (6.20 mol) of pyrrolidone (NMP) and 18.08 g (0.123 mol) of p-dichlorobenzene (p-DCB). After the inside of the reaction container was sufficiently replaced with nitrogen, it was sealed under a nitrogen atmosphere.

[0190] While stirring at 400 rpm, the temperature was raised from room temperature to 200° C. over about 1 hour. At this stage, the pressure in the reaction vessel was 0.35 MPa in gauge pressure. Then, the temperature was raised from 200°C to 270°C over about 30 minutes. The pressure in the reaction container at this stage was 1.05 MPa in gauge press...

reference example 2

[0196] Reference Example 2 (Preparation of Cyclic Polyarylene Sulfide Composition)

[0197] A stainless steel autoclave equipped with a stirrer was used as a reaction vessel. In the reaction vessel, add 47% sodium hydrosulfide 118g (1 mole), 96% sodium hydroxide 42.3g (1.01 mole), N-methyl-2-pyrrolidone (NMP) 163g (1.66 mole), sodium acetate 24.6g (0.30 mol) and 150 g of ion-exchanged water. The reaction vessel was cooled to 160°C after gradually heating to 240°C over about 3 hours under normal pressure while blowing nitrogen gas and distilling off 212 g of water and 4.0 g (40.4 mmol) of NMP. The amount of hydrogen sulfide scattered was 25 mmol.

[0198] Next, 147 g (1.00 mol) of p-dichlorobenzene (p-DCB) and 129 g (1.30 mol) of NMP were further added, and the reaction container was sealed in nitrogen atmosphere. While stirring at 400 rpm, the temperature was raised from 200°C to 270°C at a rate of 0.6°C / min, and the reaction was continued at 270°C for 140 minutes. Then, w...

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Abstract

A polyarylene sulfide containing reactive functional groups with a narrow dispersity and low amount of generated gas is produced by heating a cyclic polyarylene sulfide composition in the presence, with respect to 1 mole of arylene sulfide structural units, of 0.1 mole% to 25 mole% of a sulfide compound having reactive functional groups selected from amino groups, carboxyl groups, hydroxyl groups, acid anhydride groups, isocyanate groups, epoxy groups, silanol groups and alkoxysilane groups.

Description

technical field [0001] The present invention relates to a method for producing polyarylene sulfide having functional groups. Background technique [0002] Polyarylene sulfide represented by polyphenylene sulfide (hereinafter, sometimes abbreviated as PPS) has excellent heat resistance, barrier properties, chemical resistance, electrical insulation, heat and humidity resistance, flame retardancy, etc. Resins of the nature suitable for plastics. In addition, it can be molded into various molded parts, films, sheets, fibers, etc. by injection molding or extrusion molding, and is widely used in various electrical and electronic parts, mechanical parts, and automotive parts that require heat resistance and chemical resistance. field. [0003] As a specific production method of the polyarylene sulfide, a method of reacting an alkali metal sulfide such as sodium sulfide with a polyhalogenated aromatic compound such as p-dichlorobenzene in an organic amide solvent such as N-methyl...

Claims

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Application Information

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IPC IPC(8): C08G75/02C08G75/06
CPCC08G75/02C08G75/14C08L81/02C08L81/04
Inventor 鹿又昭纪堀内俊辅海法秀山内幸二
Owner TORAY IND INC
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