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A kind of tetrafluoroethylene and ethylene copolymer emulsion and preparation method thereof

A technology of ethylene copolymer and tetrafluoroethylene, which is applied in the field of preparation of self-emulsifying tetrafluoroethylene and ethylene copolymer emulsion, can solve problems such as the destruction of atmospheric ozone layer, unfavorable environmental protection and human health, and restricting the development of ETFE synthesis by solution method. , to achieve the effect of reducing crystallinity, improving tear resistance and good stability

Active Publication Date: 2016-06-08
SHANDONG HUAFU FLUORO CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both methods have disadvantages, which are not conducive to environmental protection and personal health.
In order to enhance the solubility of fluorine-containing elastomers, the solution polymerization method uses chlorofluoroalkanes such as trifluorotrichloroethane (F-113) as solvents. These solvents have a serious damage to the atmospheric ozone layer and are banned in developed countries, including my country. Such substances are used as solvents, which limits the development of solution synthesis of ETFE

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 10 liters of ion-free water to a 20-liter high-pressure polymerization kettle, add 1 mol of undecylenic acid and 1 mol of sodium hydroxide, vacuumize and replace the oxygen in the autoclave with nitrogen, heat up the temperature of the polymerization kettle to 50°C, and control the feeding valve to add The initial monomer of tetrafluoroethylene ethylene with a molar ratio of 45 / 55, until the internal pressure of the reactor is 3Mpa. Use a metering pump to add 30 ml of 5% initial initiator potassium persulfate aqueous solution, start polymerization, open the additional monomer (tetrafluoroethylene and ethylene molar ratio is 39 / 61) feed valve to continuously add monomer, open the additional The initiator metering pump continuously replenishes the initiator, adjusts the flow rate of the metering pump, finishes 350 ml of 5% potassium persulfate solution within 4 hours of polymerization time, controls the cooling water flow rate, and maintains the polymerization temperat...

Embodiment 2

[0017] Add 10 liters of ion-free water to a 20-liter high-pressure polymerization kettle, add 240 grams of undecylenic acid and 55 grams of sodium hydroxide, vacuumize and replace the oxygen in the autoclave with nitrogen, and the temperature of the polymerization kettle is raised to 60 ° C. Control the feeding The valve feeds the initial tetrafluoroethylene ethylene monomer with a molar ratio of 50 / 50 until the internal pressure of the reactor is 3.2Mpa. Use a metering pump to add 30 ml of 5% initial initiator potassium persulfate aqueous solution to start polymerization, open the additional monomer (tetrafluoroethylene and ethylene molar ratio is 40 / 60) feed valve to continuously add monomer, open the additional The initiator metering pump continuously replenishes the initiator, adjusts the flow rate of the metering pump, finishes 350 ml of 5% potassium persulfate solution within 4 hours of polymerization time, controls the flow rate of cooling water, and maintains the polyme...

Embodiment 3

[0020] Add 10 liters of ion-free water to a 20-liter high-pressure polymerization kettle, add 60 grams of crotonic acid and 50 grams of sodium hydroxide, vacuumize and replace the oxygen in the autoclave with nitrogen, heat the polymerization kettle to 70 ° C, and control the feeding valve to add The initial monomer of tetrafluoroethylene ethylene with a molar ratio of 48 / 52, until the internal pressure of the reactor is 3.5Mpa. Use a metering pump to add 35 ml of 5% initial initiator potassium persulfate aqueous solution, start polymerization, open the additional monomer (tetrafluoroethylene and ethylene molar ratio is 41 / 59) feed valve to continuously add monomer, open the additional The initiator metering pump continuously replenishes the initiator, adjusts the flow rate of the metering pump, finishes 350 ml of 5% potassium persulfate solution within 4 hours of polymerization time, controls the flow rate of cooling water, and maintains the polymerization temperature at 70°C ...

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Abstract

The present invention describes a self-emulsifying ethylene (E) and tetrafluoroethylene (TFE) copolymer (ETFE) emulsion and its preparation method. The polymerization is carried out in a high-pressure polymerization kettle. First add a certain amount of ion-free water to the autoclave, add a certain amount of aliphatic olefinic acid, then vacuumize and replace the oxygen in the autoclave with nitrogen, then add a certain amount of initial monomers, and raise the temperature. After reaching a certain pressure, use a metering pump to add the initial initiator to start polymerization, open the metering pump and the gas phase material feeding valve, continuously inject additional initiator and additional monomer, maintain a constant temperature and pressure, polymerize for four hours, stop polymerization, and obtain ETFE saponified emulsion. The present invention uses aliphatic alkenoic acid as a reactive emulsifier for tetrafluoroethylene and ethylene emulsion polymerization, and the prepared tetrafluoroethylene and ethylene copolymer emulsion does not contain PFOA (perfluorooctanoic acid amine) and other substances, and has no harm to human body and environment.

Description

technical field [0001] The invention relates to a preparation method of a tetrafluoroethylene-ethylene copolymer, in particular to a preparation method of a self-emulsifying tetrafluoroethylene-ethylene copolymer emulsion. Background technique [0002] The copolymer (ETFE) of ethylene (E) and tetrafluoroethylene (TFE) is the third largest fluorine material species after polytetrafluoroethylene (PTFE) and polyvinylidene fluoride (PVDF). It is called ethylene and tetrafluoroethylene in industry. The ethylene copolymer is ETFE or F40. ETFE is a crystalline polymer that combines the advantages of polytetrafluoroethylene and polyethylene. ETFE has excellent mechanical properties, its impact resistance, hardness, cold flow resistance and creep resistance are better than PTFE and FEP, and its tensile strength is close to twice that of PTFE. ETFE has excellent dielectric properties, radiation resistance, chemical corrosion resistance, weather heat resistance and high light transmi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F214/26C08F210/02C08F220/04C08F2/30
Inventor 郭依依黄传军王延平窦圣堂张书香赵继华郭希刚张景海石养渡
Owner SHANDONG HUAFU FLUORO CHEM
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