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Preparation of ethylene-tetrafluoroethylene copolymer

A tetrafluoroethylene and copolymer technology, applied in the field of fluorine-containing polymer materials, can solve the problems of unfavorable industrial production, increase the solubility of tetrafluoroethylene and ethylene, and low solubility, and achieve the advantages of large-scale industrial production and excellent chemical resistance. Corrosive, the effect of increasing the solid content

Active Publication Date: 2008-11-12
SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the low solubility of tetrafluoroethylene and ethylene in water under normal pressure, in order to improve the gas solubility in water phase polymerization, the reaction often needs to be carried out at a pressure of several hundred atmospheres, and tetrafluoroethylene is easy to decompose under high pressure to form CF 4 And C and explosion, if large-scale industrial production will increase a lot of investment in high-voltage equipment and the corresponding investment in operation, maintenance, control and safety measures
Moreover, in order to obtain the conversion rate and reaction rate required for industrial production in water phase polymerization, the reaction often needs to be carried out at a high temperature of 70-150 °C, and the synthesized polymer loses its original excellent properties due to its relatively low molecular weight.
And the water medium is used, the obtained polymer is not wetted by the medium, and it is easy to gather and condense on the plug valve or pipeline, stirring paddle, thermocouple and the wall of the reactor, and it is not easy to clean
2) Solution precipitation polymerization in chlorofluorocarbon solvents, patents US 3528954, US 3624250, US 4123602, and US 4730029 use chlorofluorocarbons or perfluorocarbon organic solvents as reaction media, which can increase tetrafluoroethylene and ethylene in the liquid phase The solubility, the reaction rate is large, and the reaction can be carried out at a lower temperature and pressure, but during the polymerization reaction in a chlorofluorocarbon solvent, the polymer chain growth is prone to chain transfer and generates a low molecular weight polymer, and the polymer It is easy to form unstable carboxylic acid end groups, and perfluoroalkane is very expensive. In the actual production process, the solvent must be recovered, and the general recovery rate does not exceed 90-95%. Polymerization is very uneconomical
3) Tetrafluoroethylene-ethylene polymerization reaction in water-organic solvent mixed system, water and chlorofluorocarbon mixed solvent immiscible as reaction medium, oil-soluble peroxy compound as initiator, no surfactant , the suspension polymerization reaction of tetrafluoroethylene and ethylene can be carried out, the reaction is carried out in the solvent phase, the existence of water reduces the viscosity of the system, and can also be used as a heat transfer medium, but the solid content of the dispersion obtained without a dispersant is not high , and it is easy to flocculate, which is not conducive to large-scale industrial production, especially continuous production, and the performance of polymers is often affected by entraining a small amount of organic solvents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Clean and vacuumize the 10L stainless steel high-pressure reactor equipped with stirring, temperature control device, circulating heating and circulating cooling water, and replace it with nitrogen three times until the oxygen content is below 10ppm, and then vacuumize to 0.0001MPa.

[0025] 5L deionized water; 225ml perfluoropropyl vinyl ether; 1ml methanol; 190g by 100g water, 60g perfluorinated dispersant CF 3 CF 2 CF 2 (OCF(CF 3 ) CF 2 ) 2 OCF (CF 3 )COOK, 30g perfluoroether oil CF 3 O(CF 2 -CF(CF 3 )O) n (CF 2 O) m CF 3, n / m=20, the microemulsion composed of an average molecular weight of 450 is sequentially added to the reactor, the temperature is raised under stirring, and the temperature is kept stable at 60°C, and ethylene and tetrafluoroethylene with a molar ratio of 1:1 are added to the system with a compressor Mix the gas until the pressure is 2.2MPa, introduce 8ml of potassium persulfate solution with a concentration of 20g / l into the system thr...

Embodiment 2

[0028] Clean and vacuumize the 10L stainless steel high-pressure reactor equipped with stirring, temperature control device, circulating heating and circulating cooling water, and replace it with nitrogen three times until the oxygen content is below 10ppm, and then vacuumize to 0.0001MPa.

[0029] 5L deionized water; 400g hexafluoropropylene; 2ml cyclohexane; 190g by 100g water, 60g perfluorinated dispersant CF 3 CF 2 CF 2 (OCF(CF 3 ) CF 2 ) 4 OCF (CF 3 )COOK, 30g perfluoroether oil CF 3 O(CF 2 -CF(CF 3 )O) n (CF 2 O) m CF 3 , n / m=20, the microemulsion composed of an average molecular weight of 450 is sequentially added into the reactor, the temperature is raised under stirring, and the temperature is kept stable at 70°C, and ethylene and tetrafluoroethylene with a molar ratio of 2:3 are added to the system with a compressor Mix the gas until the pressure is 2MPa, introduce 5ml of potassium persulfate solution with a concentration of 20g / l into the system through ...

Embodiment 3

[0032] Clean and vacuumize the 10L stainless steel high-pressure reactor equipped with stirring, temperature control device, circulating heating and circulating cooling water, and replace it with nitrogen three times until the oxygen content is below 10ppm, and then vacuumize to 0.0001MPa.

[0033] 5L deionized water; 100g hexafluoropropylene; 1.5g chloroform; 100g perfluoropropyl vinyl ether; 190g by 100g water, 60g perfluorinated dispersant CF 3 CF 2 CF 2 (OCF(CF 3 ) CF 2 ) 6 OCF (CF 3 )COOK, 30g perfluoroether oil CF 3 O(CF 2 -CF(CF 3 )O) n (CF 2 O) m CF 3 , n / m=20, the microemulsion composed of average molecular weight 450 is added into the reaction kettle in turn, the temperature is raised under stirring, and the temperature is kept stable at 80°C, and ethylene and tetrafluoroethylene with a molar ratio of 2:3 are added to the system with a compressor Mix the gas until the pressure is 2MPa, introduce 10ml of potassium persulfate solution with a concentration o...

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Abstract

The invention discloses a method for making ethylene-tetrafluoroethylene copolymer. The method adopts a microemulsion system, and the microemulsion comprises deionized water, perfluoro ether oil, perfluoro dispersant and an auxiliary agent. The obtained ethylene-tetrafluoroethylene copolymer has thermal cracking resistance at high temperature, excellent chemical corrosion resistance and outstanding mechanical property.

Description

technical field [0001] The invention belongs to the field of fluorine-containing polymer materials, and relates to a preparation method of ethylene-tetrafluoroethylene copolymer. Background technique [0002] Ethylene-tetrafluoroethylene copolymer (ETFE or F40) was discovered in the 1940s and put into production in the United States and Japan in the 1970s. ETFE has excellent electrical properties, chemical resistance and aging resistance. Due to the introduction of ethylene, the radiation resistance is greatly improved, and the improvement of its mechanical properties is more prominent. More importantly, its processing performance is greatly improved, especially its The adhesion to the metal surface is greatly improved, so that the tight lining process of fluoroplastics and steel can be truly realized. These excellent properties make the copolymer develop rapidly as a member of high-performance engineering plastics, and are widely used in wire and cable insulation materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/26C08F2/30C08F210/02
Inventor 张永明张恒高自宏裴素朋邓文忠任洪瑞
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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