Soap-free preparation method of fluoropolymer

A technology for polymers and polymerized monomers, which is applied in the field of soap-free preparation of fluorine-containing polymers, can solve problems such as cost and process not being significantly improved, complex components, difficult separation, treatment and discharge, etc. Simple operation and less water consumption

Active Publication Date: 2021-05-25
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The CN201310744861.6 invention successfully polymerized polyvinylidene fluoride resin in a soap-free manner and applied it to the field of lithium batteries. Because it still uses a variety of liquid-phase additives, the waste liquid formed has complex components, is difficult to separate, process and discharge, and costs and the process has not been significantly improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 10L horizontal reactor, add 6L of deionized water, and purge with nitrogen for 30min until the oxygen content in the reactor is less than 20ppm; prepare a total of 250g of ammonium persulfate aqueous solution with a mass fraction of 2% for later use; Add 0.5g of perfluoroethyl vinyl ether and 5g of pentafluoroethane, then start stirring, raise the temperature in the reactor to 65°C, add vinylidene fluoride monomer until the pressure in the reactor reaches 6MPa, and use a metering pump to Add the initiator, and the adding time is 60min. Continue to add vinylidene fluoride monomer to maintain the pressure until the total amount of reaction monomer reaches 1kg, stop the reaction, and copolymerize for 155min. Recover unreacted monomers, vent to normal pressure, cool down, separate products, dry, and test.

Embodiment 2

[0027] In a 10L horizontal reactor, add 6L of deionized water, and purge with nitrogen for 30min until the oxygen content in the reactor is less than 20ppm; prepare a total of 250g of ammonium persulfate aqueous solution with a mass fraction of 0.4% for later use; Add 2.5g of perfluoroethyl vinyl ether and 0.3g of difluoroethane, then start stirring, raise the temperature in the reactor to 82°C, add vinylidene fluoride monomer until the pressure in the reactor reaches 3MPa, and measure The pump added the initiator at a constant speed, and the addition time was 75 minutes. Continue to add vinylidene fluoride monomer to maintain the pressure until the total amount of reaction monomer reaches 1kg, stop the reaction, and copolymerize for 187min. Recover unreacted monomers, vent to normal pressure, cool down, separate products, dry, and test.

Embodiment 3

[0029] In a 10L horizontal reactor, add 6L of deionized water, and purge with nitrogen for 30min until the oxygen content in the reactor is less than 20ppm; prepare a total of 250g of ammonium persulfate aqueous solution with a mass fraction of 0.04% for later use; Add 5g of perfluoroethyl vinyl ether and 0.05g of ethane, then start stirring, raise the temperature in the reactor to 90°C, add vinylidene fluoride monomer until the pressure in the reactor reaches 3MPa, and add it at a constant speed with a metering pump Initiator, adding time is 90min. Continue to add vinylidene fluoride monomer to maintain the pressure until the total amount of reaction monomer reaches 1kg, stop the reaction, and copolymerize for 199min. Recover unreacted monomers, vent to normal pressure, cool down, separate products, dry, and test.

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PUM

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Abstract

The invention relates to the technical field of fluoropolymers, in particular to a soap-free preparation method of a fluoropolymer. According to the soap-free preparation method of the fluoropolymer, water is taken as a solvent, a fluorine-containing monomer and perfluorovinyl ether are taken as polymerization monomers, and the fluoropolymer is obtained through a reaction under the combined action of a gaseous chain transfer aid and an inorganic initiator. According to the soap-free preparation method of the fluoropolymer, solid-liquid separation of an obtained polymer emulsion can be achieved in a physical and mechanical mode, and a solid can be directly dried without washing to prepare a finished product, so the manufacturing cost of the fluoropolymer is effectively reduced, and environmental protection is better realized; and the content of auxiliaries and impurities in the prepared product is smaller than 1 ppm.

Description

technical field [0001] The invention relates to the technical field of fluoropolymers, in particular to a soap-free preparation method of fluoropolymers. Background technique [0002] Fluoropolymers refer to polymers containing fluorinated main chains. Because of their excellent heat resistance, chemical resistance, weather resistance, and UV stability, they have been widely used in chemical, various fields of energy. [0003] The industrialized method for the production of fluoropolymers includes the emulsion polymerization of one or more fluorinated monomers, including monomers, dispersants, media, and important components such as initiators and chain transfer aids. Auxiliary removal. Although most of the additives can be removed through post-treatment and multiple washing processes, it is difficult to completely remove them. Containing unremoved additives will affect the performance of the polymer, and the addition and removal of additives will also increase the comple...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/22C08F216/14C08F2/38C08F4/30
CPCC08F214/222C08F216/1408C08F4/30
Inventor 唐妮王汉利杜延华吕鹏程刘德鹏王梦琪
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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