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Preparation method of carboxyl-terminated liquid fluorine polymer

A liquid fluorine and carboxyl-terminated technology, which is applied in the field of preparation and curing of carboxyl-terminated liquid fluoropolymers, can solve the problems of low yield and achieve the effect of simple process and low cost

Inactive Publication Date: 2010-06-02
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mass fraction of terminal iodine in the liquid fluoropolymer prepared by this method is between 1% and 30%. This terminal iodine is relatively active and can be converted into carboxyl groups, but the yield of this preparation method is very low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 5g of vinylidene fluoride-hexafluoropropylene copolymer (molar ratio is 80 / 20, number average molecular weight Mn=5.2×10 4 , weight average molecular weight Mw=9.0×10 5 , Intrinsic viscosity [η]=0.15 of anhydrous acetone solution with a mass concentration of 0.1% at 30° C.) was dissolved in 60 g of acetone for 12 h. Weigh 1.3g of hydrogen peroxide solution with a mass concentration of 30%, and 0.5g of potassium hydroxide and dissolve them in 4ml of water. Add hydrogen peroxide solution and potassium hydroxide solution to the system at a rate of 1 drop per second at the same time, and the color of the system change. Keep the temperature of the system at 64°C, react with stirring for 5h, and then let stand for 8h.

[0025] The supernatant in the reaction mixture was poured out, and the organic phase was washed with deionized water 4 times the volume of the organic phase until the washing liquid was clear and transparent, and no oily droplets were suspended, thereby obta...

Embodiment 2

[0028] 20g of vinylidene fluoride-hexafluoropropylene-tetrafluoroethylene copolymer (molar ratio is 65 / 15 / 20, number average molecular weight Mn=5.8×10 4 , weight average molecular weight Mw=9.4×10 5 , Intrinsic viscosity [η]=0.157 of anhydrous acetone solution with a mass concentration of 0.1% at 30° C.) was dissolved in 160 g of tetrahydrofuran for 24 h. Dissolve 1.1g of potassium hydroxide in 8ml of water and add it into the reaction system, the color of the system changes. Then add 5.7 g of 30% hydrogen peroxide solution with a mass concentration of 1 drop per second. Keep the temperature of the system at 54°C, react with stirring for 15 hours, and then let it stand for 12 hours.

[0029] The aftertreatment and washing process of the reaction system are the same as in Example 1.

[0030] 17.6 g of light yellow viscous liquid (ρ(50° C.) is 150 Pa·s) was obtained, and the intrinsic viscosity of 0.3% anhydrous acetone solution at 30° C. was 0.017. Infrared analysis showed...

Embodiment 3

[0032] Dissolve 5 g of vinylidene fluoride-hexafluoropropylene copolymer (physical parameters are the same as in Example 1) in 60 g of acetone, and dissolve for 12 hours. Weigh 0.1 g of benzyltriethylammonium chloride, add it into the reaction system, and react under stirring for 20 minutes. Weigh 0.4 g of triethylamine, add it into the reaction system at a rate of 1 drop per second, and react for 1 h under stirring. Then 0.4 g of triethylamine and 1.7 g of 30% hydrogen peroxide solution were added to the system simultaneously. Stir the reaction at 54°C for 12 hours, stop the reaction, and let the reaction system stand still for 12 hours.

[0033] The aqueous phase layer in the reaction mixture was poured out, and the remaining organic phase was washed with deionized water until the washing liquid was transparent and no oily droplets were suspended. After drying, the desired product was obtained, and then the product was dissolved in acetone again, washed with deionized wate...

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Abstract

The invention discloses a preparation method of a carboxyl-terminated liquid fluorine polymer, comprising the following steps of: dissolving a solid fluorine elastomer in an organic solvent, adding oxidant and alkali, and stirring to react for 5 to 20 hours, wherein the reaction temperature is controlled within 10 to 70 DEG C, and the reaction pressure is self-generated pressure of a system; standing for 8 to 12 hours after reaction stops, and then recovering the carboxyl-terminated liquid fluorine polymer. The preparation method has the advantages of simple and easy process, less side reactions, high production ratio and low cost. The invention also discloses a solidification method of the carboxyl-terminated liquid fluorine polymer, and the carboxyl-terminated liquid fluorine polymer is reacted with an organic compound containing two or more than two epoxide groups or polyvalent metal oxides and solidified.

Description

technical field [0001] The invention relates to a preparation and curing method of a carboxyl-terminated liquid fluoropolymer. Background technique [0002] Carboxyl-terminated liquid fluoropolymer has excellent heat resistance, oxidation resistance and chemical resistance, and can be cured into any desired shape at a lower temperature according to needs, especially suitable for bonding, surface protection and porosity under harsh conditions It is an ideal sealing material, adhesive and coating for the aviation industry. [0003] At present, carboxyl-terminated liquid fluoropolymers are mainly prepared by adding a suitable molecular weight regulator into the polymerization system of fluoroelastomers. This method is complex and cumbersome in the synthesis process, with many side reactions and intermediate products and low yield. higher cost. [0004] US Patent 3,438,953 discloses a method for preparing carboxyl-ester-terminated liquid fluoropolymers by reacting vinylidene f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/22C08F8/50C08F8/06C08G59/40C08J3/24C08L27/16C08K3/22
Inventor 齐士成刘煜李吉明
Owner BEIJING UNIV OF CHEM TECH
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