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Synthesis method of fiber-grade polyphenylene sulfide (PPS) resin

A technology of polyphenylene sulfide resin and synthesis method, which is applied in the field of synthetic polyphenylene sulfide resin, can solve the problems of difficult recycling of sodium acetate and lithium chloride, etc., and achieve the reduction of "three wastes" treatment volume, production cost and recovery rate high effect

Active Publication Date: 2014-07-02
ZHEJIANG NHU SPECIAL MATERIALS +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the traditional polycondensation reaction aids sodium acetate and lithium chloride are difficult to recycle

Method used

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  • Synthesis method of fiber-grade polyphenylene sulfide (PPS) resin
  • Synthesis method of fiber-grade polyphenylene sulfide (PPS) resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] In the 100L reactor, add N-methyl-2-pyrrolidone (hereinafter referred to as NMP) 29.74Kg (300.0mol), 40% sodium hydroxide 13.0Kg (130.0mol) and hexanoic acid 3.485Kg (30.0mol), at 300rpm Under stirring speed and nitrogen protection, heat up to 120°C at a speed of 2.0°C / min, and keep warm for 1 hour; after the heat preservation is completed, heat up to 200°C at a speed of 2.0°C / min, and remove 8.74Kg of aqueous solution (water content 97.88%) , and then lower the temperature to 130°C. Add 40% sodium hydrosulfide 14.02Kg (100.0mol), NMP 4.09Kg (41.3mol), under the same stirring speed, heat up to 200°C at a speed of 1.5°C / min, remove 9.71Kg aqueous solution (water content 86.59%), After dehydration is completed, the temperature is lowered to 160°C. At this time, the amount of sulfur in the system was 99.0 mol, and the water content was 87.8 mol.

[0049]Add 14.55Kg (99.0mol) of p-dichlorobenzene (hereinafter referred to as PDCB) and 10.38Kg (104.8mol) of NMP into the abo...

Embodiment 2

[0053] In a 100L reactor, add 29.74Kg (300.0mol) of N-methyl-2-pyrrolidone (hereinafter referred to as NMP), 11.56Kg (130.0mol) of 45% sodium hydroxide and 3.485Kg (30.0mol) of 2-ethylbutyric acid ), under the stirring speed of 100rpm and nitrogen protection, with the speed of 1.0 DEG C / min, be warming up to 90 DEG C, be incubated 3 hours; Insulation finishes, be warming up to 180 DEG C with the speed of 1.0 DEG C / min, remove 7.12Kg aqueous solution ( water content 97.23%), then lower the temperature to 110°C. Add 40% sodium hydrosulfide 14.02Kg (100.0mol), NMP 4.09Kg (41.3mol), under the same stirring speed, heat up to 180°C at a speed of 0.7°C / min, remove 9.58Kg aqueous solution (water content 87.81%), After dehydration is completed, the temperature is lowered to 140°C. At this time, the amount of sulfur in the system was 99.1 mol, and the water content was 98.8 mol.

[0054] Add 14.63Kg (99.5mol) of p-dichlorobenzene (hereinafter referred to as PDCB) and 10.28Kg (103.8mol...

Embodiment 3

[0058] In the 100L reactor, add N-methyl-2-pyrrolidone (hereinafter referred to as NMP) 27.76Kg (280.0mol), 40% sodium hydroxide 11.0Kg (110.0mol) and valeric acid 1.021Kg (10.0mol), at 200rpm Under the stirring speed of 1.5 DEG C / min and under the protection of nitrogen, the temperature was raised to 100 DEG C at a speed of 1.5 DEG C / min, and the temperature was kept for 2 hours; after the heat preservation was completed, the temperature was raised to 190 DEG C at a speed of 1.5 DEG C / min, and 7.03Kg of aqueous solution (water content 97.52% ), and then lower the temperature to 110°C. Add 30% sodium hydrosulfide 18.69Kg (100.0mol), NMP 5.69Kg (57.5mol), under the same stirring speed, heat up to 190°C at a speed of 1.5°C / min, remove 14.88Kg aqueous solution (water content 87.95%), After dehydration is completed, the temperature is lowered to 150°C. At this time, the amount of sulfur in the system was 99.0 mol, and the water content was 96.3 mol.

[0059] Add 148.4Kg (101.0mo...

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Abstract

Disclosed is a method for synthesizing a fibre-grade polyphenylene sulphide resin, comprising synthesizing via a polycondensation reaction by using a sodium hydrosulphide solution and p-dichlorobenzene as raw materials, N-methyl-2-pyrrolidone as a solvent, and a C5-C6 fatty acid salt formed by dehydration of a C5-C6 fatty acid and sodium hydroxide as an auxiliary for the polycondensation reaction. The reaction liquid is subjected to acidification and washing to obtain a white polyphenylene sulphide resin, the melt flow rate of the product is less than 125 g / 10 min, the weight-average molecular weight measured by GPC is greater than 4.2 × 104, and the whiteness is higher than 90, meeting the requirements of the fibre-grade polyphenylene sulphide resin. In the method of the present invention, the C5-C6 fatty acid salt used has good solubility in NMP and can better promote the polycondensation reaction, all of it enters a filtrate after reaction and filtration, and it is again converted into a free fatty acid through acidification with hydrochloric acid; and the C5-C6 fatty acid can co-boil with water, has low solubility in water, and can be recovered from the filtrate by the method of co-boiling with water, thereby avoiding the problem that both the auxiliary and sodium chloride are dissolved in water and cannot be separated and recovered.

Description

technical field [0001] The invention relates to a method for synthesizing polyphenylene sulfide resin, in particular to a method for synthesizing fiber-grade polyphenylene sulfide resin by using a polycondensation assistant with a special structure. Background technique [0002] Polyphenylene sulfide, also known as polyphenylene sulfide (English name Polyphenylene Sulfide, abbreviated as PPS), has a symmetrical macromolecular linear rigid structure formed by connecting benzene rings and sulfur atoms. Its molecular structural formula is: [0003] [0004] Polyphenylene sulfide is a special engineering plastic with excellent performance, and it is the first plastic after polycarbonate (PC), polyester (PET), polyoxymethylene (POM), nylon (PA) and polyphenylene oxide (PPO). It is one of the six general-purpose engineering plastics and one of the eight aerospace materials. Due to its chemical structure in which sulfur atoms and benzene rings are neatly arranged alternately, p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02
CPCC08G75/02C08G75/16
Inventor 陈志荣李沃源李浩然连明尹红周贵阳郑新凤
Owner ZHEJIANG NHU SPECIAL MATERIALS
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