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Preparation method of high-strength polychlorotrifluoroethylene

A polychlorotrifluoroethylene and chlorotrifluoroethylene technology, which is applied in the field of preparation of high-strength polychlorotrifluoroethylene, can solve the problem that it is difficult to prepare high-molecular-weight polychlorotrifluoroethylene, and it is difficult to prepare high-mechanical strength polychlorotrifluoroethylene. chlorotrifluoroethylene and other problems to achieve the effect of improving stability

Active Publication Date: 2016-07-13
CHANGSHU XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, documents such as US2613202, US2689241, and US5453477 are polymerized in a redox initiation system, and it is difficult to prepare high molecular weight polychlorotrifluoroethylene, so it is difficult to prepare high mechanical strength polychlorotrifluoroethylene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a 5-liter vertical SUS316L stainless steel polymerization reactor, add 2 kg of deionized water, 2 kg of 1,1-dihydro-perfluoro-1-heptanol, and 0.6 g of 2,2-dihydro-perfluoro-ammonium heptanoate , 1.2 grams of bis(1,1-dichloro-perfluorobutyl) peroxide, the stirring speed is controlled to be 250 rpm, after deoxidation treatment, the inner temperature of the polymerization kettle is controlled at -10°C, and trifluorochlorine is continuously introduced Ethylene gas, so that the pressure in the kettle is 0.2MPa. When accumulatively 1.2 kilograms of chlorotrifluoroethylene monomers were added into the polymerization kettle, the feeding of chlorotrifluoroethylene was stopped, and the reaction was finished after 1 hour. The total polymerization time was 12 hours. The residual chlorotrifluoroethylene gas in the kettle is recovered, the pressure of the kettle is reduced to normal pressure, and the polymerized polychlorotrifluoroethylene is released to be fully washed and dried...

Embodiment 2

[0016] In a 5-liter vertical SUS316L stainless steel polymerization reactor, add 3 kg of deionized water, 2 kg of 1,1-dihydro-perfluoro-1-heptanol, and 0.15 g of 2,2-dihydro-perfluoro-ammonium heptanoate , 0.75 g of bis(1,1-dichloro-perfluorobutyl) peroxide, the stirring speed is controlled to be 250 rpm, after deoxidation treatment, the inner temperature of the polymerization kettle is controlled at -5°C, and trifluorochloro Ethylene gas, so that the pressure in the kettle is 0.24MPa. When accumulatively 1.57 kilograms of chlorotrifluoroethylene monomers were added into the polymerization kettle, the feeding of chlorotrifluoroethylene was stopped, and the reaction was finished after 1 hour. The total polymerization time was 12 hours. The residual chlorotrifluoroethylene gas in the kettle is recovered, the pressure of the kettle is reduced to normal pressure, and the polymerized polychlorotrifluoroethylene is released to be fully washed and dried to obtain a finished product....

Embodiment 3

[0019] In a 5-liter vertical SUS316L stainless steel polymerization reactor, add 2.5 kg of deionized water, 2 kg of 1,1-dihydro-perfluoro-1-heptanol, and 1.57 g of 2,2-dihydro-perfluoro-ammonium heptanoate , 1.18 grams of bis(1,1-dichloro-perfluorobutyl) peroxide, the stirring speed is controlled to be 250 rpm, after deoxidation treatment, the internal temperature of the polymerization kettle is controlled at -7°C, and trifluorochlorine is continuously introduced Ethylene gas, so that the pressure in the kettle is 0.224MPa. When accumulatively 1.57 kilograms of chlorotrifluoroethylene monomers were added into the polymerization kettle, the feeding of chlorotrifluoroethylene was stopped, and the reaction was finished after 1 hour. The total polymerization time was 12 hours. The residual chlorotrifluoroethylene gas in the kettle is recovered, the pressure of the kettle is reduced to normal pressure, and the polymerized polychlorotrifluoroethylene is released to be fully washed ...

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Abstract

The invention discloses a preparation method of high-strength polychlorotrifluoroethylene. The method adopts chlorotrifluoroethylene as a monomer, uses deionized water and 1,1?dihydro?perfluoro?1?heptanol as a medium, In the presence of 2,2?dihydro?perfluoroammonium heptanoate, bis(1,1?dichloro?perfluorobutyl) peroxide was used as an initiator to polymerize chlorotrifluoroethylene at a temperature of ? 10~?5℃; the dosage of chlorotrifluoroethylene is 30~35% of the weight of the mixed medium, and the weight ratio of deionized water and 1,1?dihydro?perfluoro?1?heptanol is 1~1.5 : 1. The amount of the bis(1,1?dichloro?perfluorobutyl) peroxide initiator is 0.05-0.1% of the weight of chlorotrifluoroethylene, 2,2?dihydro?perfluoroammonium heptanoate The dosage is 0.01-0.1% of the weight of chlorotrifluoroethylene; the polychlorotrifluoroethylene prepared by the method of the present invention has relatively high molecular weight and high mechanical strength.

Description

technical field [0001] The invention relates to a preparation method of high-strength polychlorotrifluoroethylene, which belongs to the technical field of fluorine monomer polymerization. Background technique [0002] Polytrifluorochloroethylene is a fluorine material with excellent performance, which has excellent oxygen barrier performance, so it is usually used as a packaging film for medicine. In addition, polytrifluoroethylene is used as refrigeration equipment parts, valves (valve seats, valve stems, seals), sealing materials (covers, O-rings, V-rings, special structural seals), parts of compressors and pumps, food and medicine Packaging films, liners, bearings and ordinary special-shaped parts, etc. These application fields require polychlorotrifluoroethylene to have high strength mechanical properties. [0003] At present, US patents US2613202, US2689241, US5453477 and other documents are polymerized in a redox initiation system, and it is difficult to prepare high...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F114/24C08F4/34
Inventor 窦建华陶惠平徐卫
Owner CHANGSHU XINHUA CHEM