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A kind of bio-based degradable hyperbranched epoxy resin and preparation method thereof

An epoxy resin and bio-based technology, which is applied in the direction of epoxy resin coating, coating, plastic recycling, etc., can solve the problems of unfavorable sustainable development and difficult degradation of epoxy resin, and achieve low viscosity, low raw material cost, and easy preparation The effect of simple process

Active Publication Date: 2022-05-17
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to solve the problem of difficult degradation of epoxy resin, the applicant's research group invented degradable hyperbranched epoxy resin containing hexahydro-s-triazine structure (ZL201810387204.3, ZL201810386063.3), but the raw materials of these routes are relatively short-term Based on the oil route of China, it is not conducive to the sustainable development of the industry

Method used

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  • A kind of bio-based degradable hyperbranched epoxy resin and preparation method thereof
  • A kind of bio-based degradable hyperbranched epoxy resin and preparation method thereof
  • A kind of bio-based degradable hyperbranched epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] A bio-based degradable hyperbranched epoxy resin, the preparation method steps are as follows:

[0053] Add 0.4mol of trimethylolpropane and 0.3mol of 2,5-furandicarboxylic acid to a four-necked flask equipped with a condenser, stirrer, water separator and thermometer in sequence, then add 100g of xylene and 0.5g of p- Toluenesulfonic acid. in N 2 Under the atmosphere, heat to 140°C and stir for 20 hours to react. The test acid value is about 9 mgKOH / g to stop the reaction, and the temperature is lowered to 100°C. Add 0.7mol thioglycolic acid, stir and react at 100°C for 20 hours under N2 atmosphere, and remove the water-carrying agent and excess thioglycolic acid in vacuum while hot. Then add 45g of dioxane and 45g of dichloromethane, after fully dissolving, gradually lower the temperature to room temperature. Then add 0.5g benzophenone and 0.7mol glycidyl methacrylate, react under 800W ultraviolet light for 20 minutes at room temperature, and vacuum out the organic...

Embodiment 2

[0055] A bio-based degradable hyperbranched epoxy resin, the preparation method steps are as follows:

[0056] Add 0.1mol trimethylolpropane and 0.09mol dimethyl 2,5-furandicarboxylate successively into a four-necked flask equipped with a condenser, agitator, water separator and thermometer, then add 40g xylene, 40g toluene, 0.65g tetrabutyl titanate. Heat to 170°C under N2 atmosphere and stir for 10 hours to react. The test acid value is about 8 mgKOH / g to stop the reaction, and the temperature is lowered to 120°C. Add 0.15mol mercaptopropionic acid, in N 2 Under atmosphere, stir and react at 120°C for 10 hours, remove the water-carrying agent and excess mercaptopropionic acid in vacuum while hot. Then add 13g of toluene and 15g of tetrahydrofuran, after fully dissolving, gradually lower the temperature to room temperature. Then add 0.03g of 2-methyl-1-[4-(methylthio)phenyl]-2-(4-morpholino)-1-acetone and 0.15mol glycidyl acrylate, at room temperature React with 3000W ult...

Embodiment 3

[0058] A bio-based degradable hyperbranched epoxy resin, the preparation method steps are as follows:

[0059] Add 0.22mol of trihydroxyethyl isocyanurate and 0.21mol of dibutyl 2,5-furandicarboxylate into a four-necked flask equipped with a condenser, agitator, water separator and thermometer in sequence, and then add 260g xylene, 1.25g zinc acetate. Heat to 160°C under N2 atmosphere and stir for 15 hours to react. The test acid value is about 9 mgKOH / g to stop the reaction, and the temperature is lowered to 110°C. Add 0.4mol mercaptopropionic acid, in N 2 Stir and react at 115°C for 15 hours under atmosphere, remove the water-carrying agent and excess mercaptopropionic acid in vacuum while hot. Then add 100g of dioxane and 80g of ethyl acetate, and after fully dissolving, gradually lower the temperature to room temperature. Then add 0.5g of 2-methyl-1-[4-(methylthio)phenyl]-2-(4-morpholino)-1-propanone and 0.33mol allyl glycidyl ether, at room temperature Under the condi...

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Abstract

The invention discloses a bio-based degradable hyperbranched epoxy resin and a preparation method thereof. The preparation method of the bio-based degradable hyperbranched epoxy resin of the present invention has a simple process, and the obtained bio-based degradable hyperbranched epoxy resin has the functions of degradable and toughened bisphenol A type epoxy resin, and is easy to degrade, It is expected to be used in the preparation of high-performance degradable epoxy resin and its composite materials and in the fields of degradable coatings and the like.

Description

technical field [0001] The invention relates to the technical field of hyperbranched epoxy resin and its preparation method. More specifically, the present invention relates to a bio-based degradable hyperbranched epoxy resin and a preparation method thereof. Background technique [0002] The research on the synthesis of hyperbranched epoxy resin originated in 1993. PCT International Application Patent (WO9317060) disclosed the technology of esterification reaction to synthesize hyperbranched epoxy resin. Subsequently, the inventor of the present application (Zhang Daohong) invented nitrogen-heterocyclic hyperbranched epoxy resins and silicon-skeleton hyperbranched epoxy resins with high heat-resistant temperatures (ZL200910029024.9, ZL200910029026.8, ZL200910062871.5, ZL201010224451.5). The preparation technology of the hyperbranched epoxy resin of these reports usually needs to add a large amount of organic solvents, and after the reaction is completed, most of the techni...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/32C08G59/30C09D163/00
CPCC08G59/3263C08G59/302C09D163/00C08G2230/00Y02W30/62
Inventor 陈苏芳陈显超张道洪卢燕芬张俊珩
Owner WUHAN INSTITUTE OF TECHNOLOGY
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