Method of preparing polyphenylene sulfide with synthesis mother solution

A technology for synthesizing mother liquor and polyphenylene sulfide, applied in the field of polymer materials, can solve the problems of high manufacturing energy consumption and high cost of synthesizing PPS, and achieve the effects of solving high manufacturing energy consumption, solving high cost and reducing production cost

Active Publication Date: 2017-06-27
四川中科兴业高新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] The invention provides a method for preparing polyphenylene sulfide by using synthetic mother liquor, wherein the synthetic mother liquor is the mother liquor produced in the previous

Method used

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  • Method of preparing polyphenylene sulfide with synthesis mother solution
  • Method of preparing polyphenylene sulfide with synthesis mother solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Taking the dosage of 100Kg 1,4-p-dichlorobenzene as an example, the specific operations are as follows:

[0041] (1) Feeding: first add 630kg of synthetic mother liquor into the dehydration kettle, start stirring, and then put 114.4kg of sodium sulfide pentahydrate, 2.1kg of sodium hydroxide, 7kg of lithium chloride and sodium acetate into the dehydration kettle , seal the feeding port, and pass in nitrogen protection;

[0042] (2) Dehydration: Start to heat up the reactor. When the temperature in the reactor rises to about 130°C, dehydration begins. When the dehydration amount reaches the specified requirements, the dehydration ends; during dehydration, the total amount of dehydration condensate is checked every 10 minutes Measure, and sample and analyze the dehydration condensate from the dehydration condenser until the dehydration is completed when the dehydration amount meets the specified requirements;

[0043] (3) Dissolution of 1,4-p-dichlorobenzene: 100kg of 1,4-...

Embodiment 2

[0049] According to the operation steps described in Example 1, repeat 3 times, the average molecular weights of the polyphenylene sulfide obtained 3 times are respectively: 26800, 26870, 26850, the molecular weight is high and relatively stable, indicating that the method has good stability and reproducibility The quality of the finally obtained polyphenylene sulfide is: 63.3Kg, 62.2Kg, 62.4Kg respectively, the theoretical yield is 73.578Kg, the yield of 3 repeated operations is the lowest 87.03%, and the conversion rate is high.

[0050] The physical properties of the polyphenylene sulfide obtained by repeating the operation three times are shown in Table 1:

[0051] Table 1 Physical properties of polyphenylene sulfide

[0052]

[0053] It can be seen from Table 1 that the polyphenylene sulfide prepared by the method of the present invention has excellent mechanical properties and high repeatability.

Embodiment 3

[0055] Carry out 6 groups of control experiments, be respectively compiled into 1,2,3,4,5,6, 6 groups of control experiments change lithium chloride, sodium acetate mixture as catalyzer into lithium chloride, sodium acetate respectively in embodiment 1 , sodium phosphate, sodium carbonate, caprolactone and sodium benzoate, all the other steps and conditions are the same, and the molecular weights of the obtained polyphenylene sulfide products are respectively 26830, 26840, 26820, 26860, 26830, 26850, and the polyphenylene sulfide obtained in Example 1 The molecular weight of sulfide product is consistent, and the kind of catalyzer among the present invention has little influence on the molecular weight of polyphenylene sulfide product, records remaining physical property as table 2:

[0056] Table 2 Effects of catalyst types on the physical properties of polyphenylene sulfide

[0057]

[0058] Based on the data in Table 1 and Table 2, the type of catalyst in the present inv...

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Abstract

The invention discloses a method of preparing polyphenylene sulfide with a synthesis mother solution and relates to the field of high polymer materials. Sodium sulfide and p-dichlorobenzene are taken as raw materials; the synthesis mother solution is taken as a solvent; sodium hydroxide is taken as an assistant. Particularly, the method sequentially comprises the steps of feeding, dehydration, 1,4-p-dichlorobenzene dissolution, dropwise adding, pre-polymerization, filtering, washing, drying and package to form a polyphenylene sulfide product at last. The method takes the synthesis mother solution as the solvent; the dosage of pure N-methyl pyrrolidone in a polyphenylene sulfide resin synthesis process can be reduced; the recovery cost is greatly lowered; low molecular weight polyphenylene sulfide resin in the synthesis mother solution, sodium sulfide and 1,4-p-dichlorobenzene carry out polymerization reaction again by the action of a catalyst; the waste of the low molecular weight polyphenylene sulfide resin is reduced in a recovery process of the synthesis mother solution; the synthesis mother solution also contains a certain amount of catalyst; the dosage of the catalyst is reduced in the synthesis process, so that the production cost is further lowered.

Description

technical field [0001] The invention relates to the field of polymer materials, and more specifically relates to a method for preparing polyphenylene sulfide with synthetic mother liquor. Background technique [0002] Polyphenylene sulfide has excellent thermal stability, chemical stability, corrosion resistance and electrical properties, and has good affinity with various inorganic fillers. It can be compounded with various inorganic fillers and other polymer materials to make Various engineering plastics and blended alloys with excellent performance. In addition, polyphenylene sulfide (PPS) products have outstanding dimensional stability, and can be processed by almost all plastic processing methods, including spraying, injection molding, compression molding, extrusion, blowing and potting, etc., and the products can also be processed Secondary processing. Therefore, polyphenylene sulfide (PPS) has a wide range of applications in automobile manufacturing, electrical and ...

Claims

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Application Information

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IPC IPC(8): C08G75/0213C08G75/0254C08G75/025
CPCC08G75/0213C08G75/025C08G75/0254
Inventor 刘洪陈培龙周燕李玉凤
Owner 四川中科兴业高新材料有限公司
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