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Ethylene-tetrafluoroethylene copolymer and preparation method and application thereof

A technology of tetrafluoroethylene and copolymers, applied in the field of fluorine-containing polymer materials, can solve the problems of application limitations, poor adhesion to fluorine-free polymers, insufficient stress cracking resistance of copolymers, etc., and achieve good adhesion, The effect of saving polymerization reaction time and good long-term stability

Active Publication Date: 2016-11-09
SHANDONG HUAFU FLUORO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The Chinese invention patent with the application number 201110349839.2 discloses a method for preparing a tetrafluoroethylene-ethylene copolymer. In this invention, propylene is selected as the third monomer to prepare the ethylene-tetrafluoroethylene copolymer. Since the volume of the side chain is too small, The stress cracking resistance of the copolymer is insufficient, and the problem of brittleness under high temperature is not well solved; the Chinese patent application number 201110041370.6 discloses a highly flexible quaternary copolymer fluorine-containing resin and its preparation method and application. Its structure is composed of Ethylene, tetrafluoroethylene, perfluoroalkyl vinyl ether and 2-(perfluoropropoxy) perfluoropropyl trifluorovinyl ether, the obtained ethylene-tetrafluoroethylene copolymer has good flexibility, but The ethylene-tetrafluoroethylene prepared by the present invention has poor fuel resistance and adhesion to fluorine-free polymers, and its application in fuel hoses is limited to a certain extent

Method used

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  • Ethylene-tetrafluoroethylene copolymer and preparation method and application thereof
  • Ethylene-tetrafluoroethylene copolymer and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] The 5L stainless steel autoclave equipped with stirring device, temperature control device, electric heating, and circulating cooling water was cleaned, fully dried, evacuated, and replaced with nitrogen three times until the oxygen content was below 10 ppm, evacuated to 0.0001 MPa, and added 2.5 L of deionized water containing 50 g of sodium dodecyl sulfonate, stirred and heated to 58 ° C, after the temperature of the system was constant, slowly add the initial monomer into the system, when the pressure reached 0.9 MPa, add 2 g of water using a metering pump. Oxidized di-tert-butylcyclohexyl dicarbonate initiates a polymerization reaction, wherein the molar percentage of each raw material in the initial monomer is 75% of tetrafluoroethylene, 20% of ethylene, CF 2 =CFOCF 2 CF (CF 3 )OCF 2 CF 2 CF 3 3%, Acryloyloxyethyl succinate 2%.

[0032] After the reaction started, the additional monomer was continuously added, the pressure was maintained at 1.5 MPa, and the te...

Embodiment 2

[0035] The 5L stainless steel autoclave equipped with stirring device, temperature control device, electric heating, and circulating cooling water was cleaned, fully dried, evacuated, and replaced with nitrogen three times until the oxygen content was below 10 ppm, evacuated to 0.0001 MPa, and added 3 L of deionized water containing 420 g of sodium lignosulfonate, stirred and heated to 62° C. After the temperature of the system was constant, slowly add the initial monomer into the system, and when the pressure reached 1.2 MPa, add 3 g of peroxydicarbonate with a metering pump Di-tert-butyl cyclohexyl ester initiates a polymerization reaction, wherein the molar percentage of each raw material in the initial monomer is 80% of tetrafluoroethylene, 15% of ethylene, CF 2 =CFOCF 2 CF (CF 3 )OCF 2 CF 2 CF 3 2%, acryloyloxyethyl succinate 3%.

[0036] After the reaction started, the supplementary monomer was continuously added, the temperature was maintained at 62 ° C and the pr...

Embodiment 3

[0039] Wash it in a 5L stainless steel autoclave equipped with a stirring device, temperature control device, electric heating, and circulating cooling water, fully dry it, and then vacuumize it and replace it with nitrogen three times until the oxygen content is below 10ppm, and then vacuumize to 0.0001MPa. Add 2.8L of deionized water containing 140g of sodium dodecyl sulfonate and sodium lignosulfonate, stir and heat up to 60°C, after the temperature of the system is constant, slowly add the initial monomer into the system, when the pressure reaches 1.0MPa , using a metering pump to add 2.52g of di-tert-butyl cyclohexyl peroxydicarbonate to initiate a polymerization reaction, wherein the molar percentage of each raw material in the initial monomer is 78% of tetrafluoroethylene, 18% of ethylene, CF 2 =CFOCF 2 CF (CF 3 )OCF 2 CF 2 CF 3 3%, acryloyloxyethyl succinate 1%.

[0040] After the reaction started, the additional monomer was added continuously, the temperature wa...

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Abstract

The invention relates to the field of fluorine-containing high molecular materials, in particular to an ethylene-tetrafluoroethylene copolymer and a preparation method thereof. The preparation method includes: (1), vacuumizing a high-pressure kettle, and adding a polymerization medium; (2), adding an initial monomer into the polymerization medium until pressure is 0.9-1.2 Mpa, heating to 58-62 DEG C, adding an initiator; (3), after reaction is started, continuously adding a replenishing monomer for equal-temperature equal-pressure polymerization, and stopping adding the replenishing monomer when adding amount of the replenishing monomer accounts for 10-14% of total mass of the polymerization medium and the replenishing monomer; (4), lowering temperature and pressure, discharging, washing materials, and drying to obtain the copolymer. The preparation method is short in polymerization time, simple to operate and easy for industrial production. The invention further provides application of the ethylene-tetrafluoroethylene copolymer in fuel hose inner layers.

Description

technical field [0001] The invention relates to the field of fluorine-containing polymer materials, in particular to an ethylene-tetrafluoroethylene copolymer and a preparation method and application thereof. Background technique [0002] Ethylene-tetrafluoroethylene copolymer (ETFE) is a melt-processable fluororesin that is used in many fields due to its excellent thermal and chemical stability, such as chemical reaction device linings, wire insulation materials, etc.; based on Ideally alternating copolymers with a 1:1 molar ratio of repeating units of ethylene monomers to repeating units based on tetrafluoroethylene monomers have a melting point of up to 295°C; the better the crystallinity of ETFE, the higher the crystallization temperature and the melt processability The worse it is, the worse the mechanical properties such as stress cracking prevention of the processed products are. In order to overcome the shortcomings of high crystallinity and cracking under very sm...

Claims

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Application Information

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IPC IPC(8): C08F214/26C08F210/02C08F216/14C08F222/16C08L27/18F16L11/04
CPCC08F214/26C08L27/18C08L2201/02C08L2203/18F16L11/04C08F210/02C08F216/14C08F222/165
Inventor 宿梅香郭依依郭希刚王延平赵淑娟
Owner SHANDONG HUAFU FLUORO CHEM
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