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Polyphenylene sulfide resin composition and method for manufacturing same

A technology of polyphenylene sulfide resin and composition, which is applied in the field of polyphenylene sulfide resin composition, can solve the problems of unstable molded product quality, low melting stability, low molecular weight components, etc., and achieve low gas generation and high viscosity Small changes and excellent processability

Inactive Publication Date: 2018-03-27
TORAY IND INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, PPS generally has a problem of low melt stability, and in particular, when producing films and fibers with a long melt residence time, there is a problem that the quality of the obtained molded product is not constant.
[0003] At present, the production method of PPS that has become the mainstream is a solution polymerization method in which an alkali metal sulfide such as sodium sulfide is reacted with a dihalogenated aromatic compound such as p-dichlorobenzene in an organic amide solvent such as N-methyl-2-pyrrolidone. However, PPS produced by this method contains a large amount of low molecular weight components, so there is a problem that the amount of gas generated during heating is large.

Method used

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  • Polyphenylene sulfide resin composition and method for manufacturing same
  • Polyphenylene sulfide resin composition and method for manufacturing same
  • Polyphenylene sulfide resin composition and method for manufacturing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0157] Hereinafter, the method of the present invention will be described more concretely using examples and comparative examples, but the present invention is not limited to these examples. In addition, the measuring method of a physical property is as follows.

[0158]

[0159] Quantification of the cyclic PPS contained in the PPS prepolymer was carried out using high performance liquid chromatography (HPLC). The measurement conditions of HPLC are as follows.

[0160] Device: LC-10Avp series manufactured by Shimadzu Corporation

[0161] Column: Mightysil RP-18GP150-4.6 (5 μm) manufactured by Kanto Chemical Co., Ltd.

[0162] Detector: photodiode array detector (270nm)

[0163] Quantification of cyclic PPS was performed from the area ratio of the sum of the detection areas of all peaks detected in the above-mentioned HPLC analysis to the sum of the detection areas of peaks derived from cyclic PPS.

[0164]

[0165] The molecular weights of the PPS resin and the resin ...

reference example 1

[0214] Preparation of the first PPS prepolymer

[0215] · Reaction in autoclave

[0216] By charging into an autoclave with a stirrer 28.1 g of 48% by weight of sodium hydrosulfide aqueous solution (0.241 moles as sodium hydrosulfide), 21.1 g of 48% by weight of sodium hydroxide aqueous solution (0.253 mole as sodium hydroxide) mol), 31.8 g (0.217 mol) of p-dichlorobenzene (p-DCB), and 600 g (6.05 mol) of N-methyl-2-pyrrolidone (NMP), thereby preparing a reaction mixture.

[0217] After replacing the inside of the autoclave with nitrogen gas, it was sealed, and the temperature was raised from room temperature to 200° C. over about 1 hour while stirring at 400 rpm. Next, the temperature was raised from 200°C to 250°C over about 0.5 hours. The pressure in the reactor at this stage was 1.0 MPa in gauge pressure. Then, the reaction mixture was heated by maintaining at 250° C. for 2 hours to cause a reaction.

[0218] A p-DCB NMP solution (a solution obtained by dissolving 3.5...

reference example 2

[0224] Preparation of the second PPS prepolymer

[0225] By charging into an autoclave with a stirrer 28.1 g of 48% by weight of sodium hydrosulfide aqueous solution (0.241 moles as sodium hydrosulfide), 21.1 g of 48% by weight of sodium hydroxide aqueous solution (0.253 mole as sodium hydroxide) mol), p-DCB 35.4g (0.241 mol), and NMP 600g (6.05 mol), thereby preparing a reaction mixture. In addition, the arylene unit (equivalent to 1 mole of sulfur atoms contained in sodium hydrosulfide charged as a thioetherification agent) with respect to 1 mole of the sulfur component in the reaction mixture (equivalent to And the amount of p-DCB) charged was 1.00 mol. After replacing the inside of the autoclave with nitrogen gas, it was sealed, and the temperature was raised from room temperature to 200° C. over about 1 hour while stirring at 400 rpm. Next, the temperature was raised from 200°C to 250°C over about 0.5 hours. The pressure in the reactor at this stage was 1.0 MPa in gau...

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Abstract

Provided is a polyphenylene sulfide resin composition, in which, when the sum of polyphenylene sulfide resins (a) to (c) is 100 wt%, the polyphenylene sulfide resin composition is obtained by blending10 to 50 wt% in total of the polyphenylene sulfide resin (b) and / or polyphenylene sulfide resin (c) with respect to 90 to 50 wt% of the polyphenylene sulfide resin (a), the polyphenylene sulfide resin composition having a viscosity change rate of no greater than 1.5 times when heated for 5 hours at 320DEG C. A PPS resin composition is provided in which there is little change in viscosity during melt retention and little gas is generated during heating, which comprises: a polyphenylene sulfide resin (a), which is polyphenylene sulfide resin having a weight average molecular weight of 50,000 ormore, having a ratio of weight loss when heated [delta]Wr, represented by formula (1), of no greater than 0.18%; a polyphenylene sulfide resin (b), which is polyphenylene sulfide resin having a weight average molecular weight of less than 50,000, in which the content of alkaline earth metals is less than 200 ppm, and the ratio of increase in molecular weight is 5.0% or less when 0.5 wt% of 2-(3,4-epoxycyclohexyl)ethyl trimethoxysilane is added and heated at 320DEG C for 10 minutes; and a polyphenylene sulfide resin (c), which is a polyphenylene sulfide resin in which the content of an alkaliearth metal (d) is 200 to 800 ppm, having a ratio of weight loss when heated [delta]Wr, represented by formula (1), of greater than 0.18%. [delta]Wr = (W1-W2) / W1 * 100 (%) ..(1) (Here, [delta]Wr isthe ratio of weight loss (%), which is a value found from the sample weight (W1) when 100DEG C is reached and the sample weight (W2) when 330DEG C is reached, when subjected to thermogravimetric analysis at a heating rate of 20DEG C / minute in a non-oxidizing atmosphere at normal pressure.)

Description

technical field [0001] The present invention relates to a polyphenylene sulfide resin composition having excellent melt stability and a small amount of gas generation, and a method for producing the same. Background technique [0002] Polyphenylene sulfide (hereinafter, may be abbreviated as PPS in some cases) has a high melting point and has properties preferable as engineering plastics, such as excellent flame retardancy and chemical resistance. PPS can be formed into various molded products, films, sheets, fibers, etc. by common melt processing methods such as extrusion molding, injection molding, and compression molding. Therefore, it has been used in electrical and electronic equipment, automotive equipment, etc. Widely used in a wide range of fields. However, PPS generally has a problem of low melt stability, and in particular, there is a problem that the quality of the obtained molded product is not constant when a film or fiber having a long melt residence time is p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0209C08L81/02
CPCC08L81/02C08G75/0209C08K3/08C08K2003/0818
Inventor 高尾英伸海法秀堀内俊辅
Owner TORAY IND INC
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