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Preparation method of biological basic characteristic type flame-retardant epoxy resin

An epoxy resin and biological technology, applied in the direction of fire-resistant coatings, etc., can solve the problems of non-renewable, poor flame-retardant performance, toxic raw materials, etc., and achieve the effect of large quantity, low price and few steps

Active Publication Date: 2020-05-29
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for preparing a bio-based flame-retardant epoxy resin in order to solve the problem that the traditional epoxy resin raw materials are toxic and non-renewable, and the flame-retardant performance is poor.

Method used

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  • Preparation method of biological basic characteristic type flame-retardant epoxy resin
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  • Preparation method of biological basic characteristic type flame-retardant epoxy resin

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preparation example Construction

[0033] A kind of preparation method of bio-basic flame-retardant epoxy resin, vanillic acid and resorcinol undergo Friedel-Crafts acylation reaction under catalytic conditions, and then undergo substitution reaction with epichlorohydrin to obtain epoxy monomer, and The curing agent DDS is mixed and cured under heating to obtain the final resin sample.

[0034] The synthesis steps of the bio-based epoxy monomer and curing agent are as follows:

[0035](1) Add a certain amount of vanillic acid, resorcinol and boron trifluoride ether into a round bottom flask with a condenser, heat to 70-120°C, and keep the mixture at this temperature for 40-120min. After cooling to room temperature, pour sodium acetate buffer solution and let it stand for 3 to 7 hours. The product was obtained by filtration, washed with water, purified by recrystallization, and then vacuum-dried at 50-80° C. for 5-9 hours to obtain the product DA. The molar ratio of vanillic acid and resorcinol is 0.7-1.5:1, t...

Embodiment 1

[0041] (1) Add 0.12 mol of vanillic acid, 0.17 mol of resorcinol and 0.36 mol of boron trifluoride ether into a round-bottomed flask with a condenser tube, heat to 120°C, and keep the mixture at this temperature for 120 min. After cooling to room temperature, pour a sodium acetate buffer solution with a mass fraction of 5%, wherein the sodium acetate is 2.4 mol, and let stand for 7 hours. The product was obtained by filtration, washed with water, purified by recrystallization from dichloromethane, and then vacuum-dried at 80° C. for 9 h to obtain the product DA.

[0042] (2) Add 0.08mol of the above-mentioned product in a round bottom flask with a condenser tube, place it under N 2 in environment. Add 0.24mol epichlorohydrin into the flask at room temperature, heat to 130°C, slowly add 10% NaOH solution within 90min, wherein the NaOH content is 0.24mol, and keep the reaction mixture at this temperature for 90min. After cooling to room temperature, the product was obtained by...

Embodiment 2

[0045] (1) Add 0.12 mol of vanillic acid, 0.17 mol of resorcinol and 0.36 mol of boron trifluoride diethyl ether into a round-bottomed flask with a condenser tube, heat to 70°C, and keep the mixture at this temperature for 40 minutes. After cooling to room temperature, pour a sodium acetate buffer solution with a mass fraction of 5%, wherein the sodium acetate is 2.4 mol, and let it stand for 3 hours. The product was obtained by filtration, washed with water, purified by tetrahydrofuran recrystallization, and then vacuum-dried at 50° C. for 5 h to obtain the product DA.

[0046] (2) Add 0.08mol of the above-mentioned product in a round bottom flask with a condenser tube, place it under N 2 in environment. Add 0.24mol epichlorohydrin into the flask at room temperature, heat to 70°C, slowly add 10% NaOH solution within 30min, wherein the NaOH content is 0.24mol, and keep the reaction mixture at this temperature for 30min. After cooling to room temperature, the product was obta...

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Abstract

The invention provides a preparation method of biological basic characteristic type flame-retardant epoxy resin. The preparation method comprises the following steps: reacting vanillic acid with resorcinol to obtain trihydric alcohol containing a benzophenone structure, further introducing an epoxy group through a phenolic hydroxyl group to obtain a bio-based epoxy monomer with a structure similarto that of DGEBA used in general industry, and mixing and curing the bio-based epoxy monomer and a curing agent under certain conditions to obtain the flame-retardant bio-based epoxy resin. The resinis wide in raw material source, environmentally friendly, simple in synthesis process, high in thermal stability and good in flame retardant property, the carbon residue amount at 800 DEG C can reach35%, the limit oxygen index can reach 34% at most, and the vertical combustion grade reaches the V-0 grade.

Description

technical field [0001] The invention relates to a method for preparing a bio-basic flame-retardant epoxy resin. Renewable bio-energy is used as a raw material, and the molecular structure of epoxy monomers is designed so that the prepared epoxy resin does not introduce flame-retardant In the absence of elements, it has good flame retardant properties. Background technique [0002] Petroleum-based plastics have various excellent properties, and can provide various raw materials and products for various industries such as construction, automobile, machinery manufacturing, electronic information, etc., and play a very important role in modern social life. With the continuous deepening of the understanding of issues such as resource crisis and other issues, the high value-added characteristics of biomass resources have also attracted increasing attention. The search for renewable biomass resources to replace petroleum products has attracted people's attention. Most biological m...

Claims

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Application Information

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IPC IPC(8): C08G59/32C08G59/50C09K21/14
CPCC08G59/3218C08G59/504C09K21/14
Inventor 潘政胡立红冯国东薄采颖李卓任晓丽周永红
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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