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Fluorine-containing epoxy resin, and preparation method and application thereof

A technology of epoxy resin and fluorine-containing alkyl group, applied in the field of fluorine-containing epoxy resin and its preparation, can solve the problems of insignificant improvement of coating hydrophobic performance and stain resistance, complicated synthesis method and high cost, and achieve excellent hydrophobic performance , the preparation method is simple, the effect of high fluorine content

Inactive Publication Date: 2014-07-30
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current fluorine-containing epoxy resin mainly adds a single or less fluorine atom to the main chain segment. Although this type of monomer can improve the heat resistance and corrosion resistance of the coating, but because of its low fluorine content, it is harmful to the coating. The hydrophobic performance and anti-fouling performance are not obviously improved, and the synthesis method is complicated and the cost is high, which limits its application range; in addition, although the compatibility can be increased by adding small molecule fluorine-containing epoxy resin, the amount of use is large , high cost, and has a certain volatility, which pollutes the environment; finally, from the perspective of technical effects, short fluorine-containing chains are difficult to migrate to the surface of the coating, which weakens the effect of fluorine-containing group modification, thus greatly limiting The scope of application of fluorine-containing epoxy coatings

Method used

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  • Fluorine-containing epoxy resin, and preparation method and application thereof
  • Fluorine-containing epoxy resin, and preparation method and application thereof
  • Fluorine-containing epoxy resin, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Mix 1g of di-n-butyl malonate, 100g of toluene, and 5g of tetrabutylammonium hydroxide aqueous solution (25% in mass fraction) evenly, react at 30°C for 3 hours, distill off the toluene under reduced pressure, and then continue to add 20g Tetrahydrofuran, 5g containing trifluoroethyl methacrylate, mixed uniformly, reacted for 0.1h, and removed tetrahydrofuran by distillation under reduced pressure to obtain the reaction product;

[0033] (2) At 80°C, mix 10g of trifluoroacetic acid and 80g of dioxane to obtain a mixed solution, add the reaction product obtained in step (1) into the mixed solution for hydrolysis for 1.5 hours, and obtain carboxyl-terminated polyformaldehyde Propylene is trifluoroethyl ester;

[0034] (3) Under the protection of nitrogen, mix 5g of carboxyl-terminated polymethacrylic trifluoroethyl ester obtained in step (2), 5g of glycidyl alcohol and 100g of tetrahydrofuran, and then continue to add 0.05g of dehydrating agent N,N '-Dicyclohexylcarb...

Embodiment 2

[0038] (1) Mix 0.1g of di-n-butyl malonate, 30g of toluene, and 0.5g of tetrabutylammonium hydroxide aqueous solution (25% by mass fraction) evenly, react at 40°C for 20h, distill off the toluene under reduced pressure, and then continue Add 10 g of tetrahydrofuran and 25 g of hexafluorobutyl acrylate, mix well, react for 3 hours, and distill off the tetrahydrofuran under reduced pressure to obtain the reaction product;

[0039] (2) At 100°C, mix 60g of trifluoroacetic acid and 100g of dioxane to obtain a mixed solution, add the reaction product obtained in step (1) into the mixed solution and hydrolyze for 0.5h to obtain carboxyl-terminated polyacrylic acid Hexafluorobutyl;

[0040] (3) Under the protection of argon, mix 30g of carboxyl-terminated polyhexafluorobutyl acrylate obtained in step (2), 20g of glycidyl alcohol and 200g of pyridine, and then continue to add 4g of dehydrating agent 1-ethyl-( 3-Dimethylaminopropyl) carbodiimide hydrochloride and 2g catalyst 6-chloro-...

Embodiment 3

[0044] (1) Mix 10g of di-n-butyl malonate, 200g of toluene, and 40g of tetrabutylammonium hydroxide aqueous solution (mass fraction: 25%) evenly, react at 50°C for 20h, distill off the toluene under reduced pressure, and then continue to add 100g Tetrahydrofuran, 100g of hexafluorobutyl methacrylate, mixed uniformly, reacted for 3h, and obtained the reaction product after removing tetrahydrofuran by distillation under reduced pressure;

[0045] (2) At 0°C, mix 30g of trifluoroacetic acid and 100g of dioxane to obtain a mixed solution, add the reaction product obtained in step (1) into the mixed solution for hydrolysis for 6 hours, and obtain carboxyl-terminated polymethyl Hexafluorobutyl acrylate;

[0046] (3) Under the protection of nitrogen, mix 50g of carboxyl-terminated polyhexafluorobutyl methacrylate obtained in step (2), 20g of glycidyl alcohol and 100g of chloroform, and then continue to add 2.5g of dehydrating agent 1- Ethyl-(3-dimethylaminopropyl)carbodiimide hydroc...

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Abstract

The invention relates to a fluorine-containing epoxy resin, and a preparation method and application thereof. The preparation method comprises the following steps: mixing di-n-butyl malonate, methylbenzene and tetrabutyl ammonium hydroxide at 30-60 DEG C to react for 1-20 hours, adding tetrahydrofuran and fluorine-containing monomer to react for 0.1-3 hours, and reacting the reaction product with trifluoroacetic acid and dioxane at 0-100 DEG C for 0.5-6 hours to obtain a carboxyl-terminated fluorine-containing polymer; and under inert-gas protection, reacting the fluorine-containing polymer with glycidol, organic solvent, dehydrating agent and catalyst at 0-100 DEG C for 1-60 hours, thereby obtaining the fluorine-containing epoxy resin. The fluorine content in the fluorine-containing epoxy resin is high; and the preparation method is simple. The fluorine-containing epoxy resin is used for preparing epoxy resin paint.

Description

technical field [0001] The invention belongs to the field of fluorine-containing epoxy coatings, and in particular relates to a fluorine-containing epoxy resin and a preparation method and application thereof. Background technique [0002] Epoxy resin coatings are widely used because of their low price, abundant sources, high hardness, good transparency and excellent mechanical and physical properties, but epoxy coatings have problems such as weather resistance and poor wear resistance, especially due to the The high surface energy limits its use in special coatings such as highly hydrophobic and antifouling, and cannot meet the surface treatment requirements of special engineering equipment and facilities. [0003] Fluorine-containing epoxy coatings have excellent properties such as corrosion resistance, weather resistance, water resistance, oil resistance, and self-cleaning, which have attracted extensive attention in the field of waterproof and antifouling coatings. The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/22C08F120/24C08F8/14C08F8/12C09D133/16
Inventor 刘伟区闫振龙
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI