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Preparation method of hyperbranched polyphenylene sulfide

A technology of polyphenylene sulfide and dichlorothiophenol, which is applied in the field of preparation of hyperbranched polyphenylene sulfide, can solve the problems of severe end group decomposition, single end-capping end group, and increased viscosity, and achieve short reaction time , good thermal stability, high molecular weight effect

Inactive Publication Date: 2019-09-20
YIBIN TIANYUAN GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In view of the fact that the end-capping end group in the prior art is relatively single, and at the same time, in the high-temperature melting process, the end-group decomposition is relatively serious, and problems such as carbonization, darkening of color, increase of viscosity, and difficulty in processing occur. The present invention provides a hyperbranched polymer The preparation method of phenylene sulfide

Method used

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  • Preparation method of hyperbranched polyphenylene sulfide
  • Preparation method of hyperbranched polyphenylene sulfide
  • Preparation method of hyperbranched polyphenylene sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A preparation method of hyperbranched polyphenylene sulfide includes the following steps:

[0033] 1. Put 2,4-dichlorothiophenol (1 part), sodium hydroxide (1.5 parts), potassium acetate (0.9 parts) into the solvent of N,N-dimethylformamide (8 parts), Put it into a three-necked flask and heat it in an oil bath under the protection of high-purity nitrogen (99.999%);

[0034] 2. Raise the temperature of the system in step 1 to 275°C for 180 minutes;

[0035] 3. Cool the system of step 2 to 80°C, add 8 parts of distilled water, and continue to stir for 60 minutes;

[0036] 4. Put the system of step 3 into 40 parts by mass of 8% hydrochloric acid solution, and continue to stir for 240 minutes;

[0037] 5. After filtering the system of step 4, take the filtrate, put it into 16 parts of acetone solution for elution, and repeat the elution 8 times;

[0038] 6. After filtering the system of step 5, take the filtrate and put it into 20 parts of distilled water for elution, and repeat the ...

Embodiment 2

[0041] A preparation method of hyperbranched polyphenylene sulfide includes the following steps:

[0042] 1. Put 2,4-dichlorothiophenol (1.1 parts), sodium hydroxide (1.6 parts), potassium acetate (1 part) into the solvent of N,N-dimethylformamide (8 parts), Put it into a three-necked flask and heat it in an oil bath under the protection of high-purity nitrogen (99.999%);

[0043] 2. Raise the temperature of the system in step 1 to 270°C for 180 minutes;

[0044] 3. Cool the system of step 2 to 85°C, add 8 parts of distilled water, and continue to stir for 60 minutes;

[0045] 4. Put the system of step 3 into 40 parts by mass of 8% hydrochloric acid solution, and continue to stir for 240 minutes;

[0046] 5. After filtering the system of step 4, take the filtrate, put it into 17 parts of acetone solution for elution, and repeat the elution 8 times;

[0047] 6. After filtering the system of step 5, take the filtrate and put it into 19 parts of distilled water for elution, and the elution...

Embodiment 3

[0050] A preparation method of hyperbranched polyphenylene sulfide includes the following steps:

[0051] 1. Put 2,4-dichlorothiophenol (1.2 parts), sodium hydroxide (1.7 parts), potassium acetate (1.1 parts) into the solvent of N,N-dimethylformamide (8 parts), Put it into a three-necked flask and heat it in an oil bath under the protection of high-purity nitrogen (99.999%);

[0052] 2. Raise the temperature of the system in step 1 to 268°C for 180 minutes;

[0053] 3. Cool the system of step 2 to 80°C, add 8 parts of distilled water, and continue to stir for 60 minutes;

[0054] 4. Put the system of step 3 into 40 parts by mass of 8% hydrochloric acid solution, and continue to stir for 240 minutes;

[0055] 5. After filtering the system of step 4, take the filtrate, put it into 18 parts of acetone solution for elution, and repeat the elution 8 times;

[0056] 6. After filtering the system of step 5, take the filtrate and put it into 18 parts of distilled water for elution, and repeat t...

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Abstract

The invention belongs to the field of high polymer materials, and particularly discloses a preparation method of hyperbranched polyphenylene sulfide. The preparation method comprises the following steps: (1) adding 2,4-dichlorothiophenol, sodium hydroxide and potassium acetate into an N,N-dimethylformamide solvent, and carrying out oil bath heating under the protection of high-purity nitrogen; (2) increasing the temperature of the system to 255-275 DEG C, and carrying out constant-temperature treatment on the system for 150-210 minutes; (3) cooling the system to 80-90 DEG C, adding distilled water, and continuously stirring the system for 30-60 minutes; (4) adding the system into a hydrochloric acid solution, and continuously stirring the system for 180-240 minutes; (5) filtering the system, and adding a filtered-out substance into an acetone solution for elution; (6) filtering the system after elution, and adding a filtered-out substance into distilled water for elution; and (7) filtering the system after elution, and drying a filtered-out substance to obtain the hyperbranched polyphenylene sulfide powder product. The preparation method is low in raw material price, simple in reaction process and short in reaction time, the synthesis process is easy to control, the reaction yield is high, and the rate of unqualified products is greatly reduced.

Description

Technical field [0001] The invention belongs to the field of polymer materials and specifically discloses a preparation method of hyperbranched polyphenylene sulfide. Background technique [0002] Polyphenylene sulfide is a white or beige, high crystallinity, hard and brittle polymer. The density of pure polyphenylene sulfide is 1.34g / cm 3 , The density will increase after compound modification, the melting point is 280~290℃, the glass transition temperature is around 110℃, and the crystallinity is generally around 65%. The thermal decomposition temperature in the air can reach up to 450°C. So far, no solvent can be found that can dissolve polyphenylene sulfide within 200°C. Polyphenylene sulfide has excellent high temperature resistance and chemical corrosion resistance. Its output ranks first in special engineering plastics, and it ranks sixth in the application of engineering plastics. It has very good application prospects and economic value. Polyphenylene sulfide is one of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C08G75/02
CPCC08G75/0209C08G75/0272C08G83/005
Inventor 罗云侯天武杨连智孙永贵
Owner YIBIN TIANYUAN GRP CO LTD
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