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Preparation method of modified polyvinylidene fluoride through chlorotrifluoroethylene

A technology of chlorotrifluoroethylene and polyvinylidene fluoride is applied in the field of preparation of chlorotrifluoroethylene-modified polyvinylidene fluoride, which can solve the problems of difficult processing of high molecular weight components, inability to effectively control molecular weight size and molecular weight distribution, and the like, To achieve the effect of excellent corrosion resistance

Active Publication Date: 2012-07-18
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the chain transfer agent is added at one time before the reaction, and the chain transfer agent is not added intermittently in batches. At the beginning of the polymerization, the content of the chain transfer agent is relatively large, and a large amount of initiator or a higher temperature is required to initiate the reaction. A large amount of low molecular weight is obtained from polymerization. As the reaction progresses, the chain transfer agent gradually decreases to obtain a certain high molecular weight. At the same time, in the later stage of the reaction, the chlorine content increases and the concentration of the initiator does not change much. , the molecular weight size and molecular weight distribution cannot be effectively controlled, and a large number of high molecular weight components are obtained, resulting in difficult processing

Method used

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  • Preparation method of modified polyvinylidene fluoride through chlorotrifluoroethylene

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Embodiment 1

[0050] The preparation of embodiment 1 PVDF-CTFE polymer

[0051] In a 50L stainless steel vertical reaction kettle, add 32kg of water, blow nitrogen and oxygen three times, evacuate until the oxygen content is less than or equal to 25ppm, add 40g of perfluorooctanoic acid, 400ml of liquid paraffin (liquid at normal temperature), start stirring, the speed is 200rpm, and the temperature is raised to 60 ℃, add 95mol% vinylidene fluoride and 5mol% chlorotrifluoroethylene to 2.5MPa, after the system is stable, add 20g of diethyl malonate to the reaction kettle through a metering pump, and add 40ml of IPP after a few minutes (Diisopropyl peroxydicarbonate) dissolved in 15ml of chlorofluorocarbon F113 (CCl 2 FCClF 2 ) into the reactor to start the polymerization reaction. At the same time, keep adding mixed monomers to keep the pressure of the reactor at 2.8MPa, and then add 10ml IPP and 20g diethyl malonate at one time for every 20% increase in conversion rate, and add 4 times un...

Embodiment 2

[0058] In a 50L stainless steel vertical reaction kettle, add 32kg of water, blow nitrogen and oxygen three times, evacuate until the oxygen content is equal to 30ppm, add 40g of sodium perfluorooctanoate, 400ml of liquid paraffin, start stirring at a speed of 200rpm, heat up to 65°C, and add 85mol% of Vinylidene fluoride and 15mol% chlorotrifluoroethylene to 2.5MPa, after the system is stable, 15g of diethyl malonate is added to the reactor by a metering pump, and 40ml of IPP (dicarbonate peroxide) is added to the reactor after a few minutes. isopropyl ester) dissolved in 15ml chlorofluorocarbon F113 (CCl 2 FCClF 2 ) into the reactor to start the polymerization reaction. At the same time, continue to add mixed monomers to keep the pressure of the reactor at 2.8 MPa, and then add 15ml IPP and 15g diethyl malonate at one time for every 20% increase in conversion rate, add 4 times, recover unreacted monomers, and obtain PVDF-CTFE Polymer 15.4Kg. Coagulate the obtained polymer...

Embodiment 3

[0064] In a 50L stainless steel vertical reaction kettle, add 32kg of water, blow nitrogen and oxygen three times, evacuate until the oxygen content is less than or equal to 30ppm, add 40g of ammonium perfluorooctanoate, 400ml of liquid paraffin, start stirring at a speed of 200rpm, heat up to 60°C, and add 80mol% Vinylidene fluoride and 20mol% chlorotrifluoroethylene to 2.8MPa, after the system is stable, after the diethyl malonate of 20g is added to the reactor by a metering pump, 40ml of IPP (diisoperoxydicarbonate Propyl ester) dissolved in 15ml chlorofluorocarbon F113 (CCl 2 FCClF 2 ) into the reactor to start the polymerization reaction. At the same time, continue to add mixed monomers to keep the pressure of the reactor at 2.8 MPa, and then add 12ml IPP and 15g diethyl malonate at one time for every 20% increase in conversion rate, add 4 times, recover unreacted monomers, and obtain PVDF-CTFE Polymer 15Kg. Coagulate the obtained polymer in frozen brine at -45°C, thaw...

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Abstract

The invention relates to a preparation method of modified polyvinylidene fluoride through trifluorochlor oethylene and applications of the modified polyvinylidene fluoride. The preparation method comprises the steps of a) adding the mixture of gas monomers of vinylidene fluoride and chlorotrifluoroethylene into an aqueous medium containing a fluorinated emulsifier so as to form dispersoid; b) then adding an organic peroxide initiator and a chain transfer agent in the dispersoid obtained from the step a); and c) adjusting and supplementing polymerization monomers, controlling the content of the chlorotrifluoroethylene, keeping gas phases in a kettle to be constant relatively, and stopping reaction until the solid content of the emulsion in a reactor to be 30%.

Description

technical field [0001] The invention relates to a preparation method of polyvinylidene fluoride modified by chlorotrifluoroethylene. Background technique [0002] PVDF (polyvinylidene fluoride) resin has excellent chemical resistance, product stability, high temperature resistance, weather resistance, ultraviolet resistance and high-energy radiation; in addition, PVDF also has excellent electrical insulation, non-hygroscopicity and self-extinguishing properties; Vinyl fluoride homopolymer or copolymer also has unique piezoelectricity and pyroelectricity. In order to make PVDF more suitable for harsh service conditions, it is necessary to improve the flexibility, elongation at break and impact strength of PVDF homopolymer. For this reason, the method of blending is used to mix vulcanized rubber into PVDF resin for extrusion processing to obtain products with good impact resistance; the method of copolymerization can also be used to modify the homopolymer. Usually, the PVDF ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/22C08F214/24C08F2/30C08F6/22
Inventor 王先荣李斌刘斌张建新赵少春高家勇兰军
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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