Preparation method of fluorine-containing polymer

A technology for polymers and fluorine-containing olefins, which is applied in the field of preparation of fluorine-containing polymers, and can solve problems such as high risk, affecting the polymerization process and polymer performance, and high risk in the preparation process

Inactive Publication Date: 2012-06-20
JUHUA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] DuPont uses the perfluoroalkyl iodide telomerization method to prepare various surfactants containing hydrocarbon segments in the molecular chain. As a substitute for PFOA, the preparation process is complicated and dangerous. It is used for fluorine-containing During the preparation method of polymer emulsion, the hydrocarbon segment in the molecular segment has the possibility of chain transfer phenomenon, which affects the polymerization process and polymer performance; 3M company adopts acyl fluoride telomerization method and perfluoroalkyl vinyl ether Raw materials are used to prepare surfactants containing ether bond segments in a variety of molecular chains. As a substitute f

Method used

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  • Preparation method of fluorine-containing polymer
  • Preparation method of fluorine-containing polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Taking a 5L polymerization kettle as an example, add 2.97L deionized deoxygenated water, 3g fluorine-containing surfactant CF 2 ClCFClOCF 2 CF(CF 3 )OCF 2 CF 2 SO 3 NH 4 , and then vacuumize and remove oxygen until the oxygen content in the polymerization tank is ≤ 20ppm, which is qualified. Use tetrafluoroethylene monomer to increase the pressure of the polymerization tank to 2.0MPa. After the temperature of the polymerization tank rises to 75°C, add the concentration of 30ml of 10% ammonium persulfate aqueous solution, start the polymerization reaction, keep the temperature at 75°C, and keep the pressure at 2.0MPa. After 12 hours of reaction, stop adding monomer, and when the pressure drops to 0.5MPa, recover unreacted tetrafluoroethylene . Agglomerated, washed, and dried to obtain 670 g of polytetrafluoroethylene solid powder.

Embodiment 2

[0025] Taking a 5L polymerization kettle as an example, add 2.9L deionized deoxygenated water, 0.3g fluorine-containing surfactant ClCF 2 (CF 2 ) 5 OCF 2 CF 2 SO 3 K, then vacuumize and remove oxygen until the oxygen content in the polymerization tank is ≤ 20ppm, it is qualified, use vinylidene fluoride monomer to increase the pressure of the polymerization tank to 6.0MPa, and when the temperature of the polymerization tank rises to 45°C, add 15g Diisopropyl peroxydicarbonate, start the polymerization reaction, keep the temperature at 45°C, and add vinylidene fluoride monomer in time according to the polymerization reaction process, so that the pressure in the kettle is kept at 6.0MPa, and stop after 10 hours of reaction Add monomer, when the pressure drops to 0.5MPa, recover unreacted vinylidene fluoride. Agglomerated, washed, and dried to obtain 600 g of polyvinylidene fluoride solid powder.

Embodiment 3

[0027] Take a 5L polymerization kettle as an example, add 3L deionized deoxygenated water, 15g fluorine-containing surfactant CF 2 ClCFClOCF 2 CF(CF 3 )OCF 2 COONa, 100g perfluoropropyl vinyl ether, and then vacuumize and remove oxygen until the oxygen content in the polymerization kettle is ≤ 20ppm, which is qualified. Use tetrafluoroethylene monomer to boost the pressure of the polymerization kettle to 1.0MPa, and wait for the temperature of the polymerization kettle to rise. After reaching 25°C, use a metering pump to add 30g bisperfluoroacyl peroxide to start the polymerization reaction, keep the temperature at 25°C, and keep the pressure at 1.0MPa. After 15 hours of reaction, stop feeding and recover unreacted tetrafluoroethylene and perfluoropropyl vinyl ether. Agglomerated, washed, and dried to obtain 550 g of modified polytetrafluoroethylene solid powder.

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Abstract

The invention discloses a preparation method of fluorine-containing polymer. The fluorine-containing polymer is obtained through the emulsion polymerization of fluorine-containing olefins monomer in the aqueous medium of fluorine-containing surfactant under the existence of initiator, wherein the weight percentage concentration of the fluorine-containing surfactant in the aqueous medium is 0.01-1%, the weight percentage concentration of the initiator in the aqueous medium is 0.001-1%, the reaction temperature is 10-120 DEG C and the pressure is 1-6.5MPa, and the reaction time is 3-15hours. The fluorine-containing surfactant satisfies a general formula shown in the specifications, wherein a is equal to 0 or 1; b is equal to 1 or 2; c is equal to 1, 2 or 3; d is equal to 1 or 2; X is C1, F or CF3; Y is H, F or CF3; and M is carboxylate or sulphonate. According to the method, perfluoro caprylic acid and derivatives thereof are not used in the method, so the method is environment-friendly; the preparation process can be conducted under wild temperature and pressure condition without affecting the reaction ratio of the polyreaction; and polymer powder with multiple grain sizes can be obtained, and thereby fluorine-containing polymer products at various grades can be prepared.

Description

technical field [0001] The invention relates to a preparation method of a fluorine-containing polymer, in particular to a preparation method of a fluorine-containing polymer not containing perfluorooctanoic acid and its salt. Background technique [0002] The emulsion polymerization method of fluorine-containing olefins and copolymerized modified monomers has the advantages of fast polymerization rate, good copolymerization performance, small particle size in the resulting dispersion, high polymerization yield, and good dispersion stability. , is a more commonly used polymerization method for polymerizing fluoromonomers into fluoropolymers. Perfluorooctanoic acid and its salts (PFOA) are the most commonly used fluorosurfactants in the emulsion polymerization of fluoromonomers. However, because of their potential bioaccumulation, toxicity and regional diffusion, they have been approved by Switzerland, the European Union and the United States successively. etc. Restricted use...

Claims

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Application Information

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IPC IPC(8): C08F14/18C08F2/24C08F114/26C08F114/22C08F214/26C08F214/28
Inventor 付铁柱王树华张士林
Owner JUHUA GRP
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