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A kind of resveratrol-based flame retardant epoxy resin and preparation method thereof

A technology of epoxy resin and resveratrol, applied in the field of resveratrol-based flame retardant epoxy resin, can solve the problems of poor flame retardancy, high toxicity of raw materials, non-renewable, etc., and achieves improved flame retardant performance, cross-linking high density effect

Active Publication Date: 2022-02-08
NANJING UNIV
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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 an all-bio-based flame-retardant epoxy resin in order to solve the problems that traditional synthetic resins have poor flame retardancy and raw materials are highly toxic and non-renewable

Method used

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  • A kind of resveratrol-based flame retardant epoxy resin and preparation method thereof
  • A kind of resveratrol-based flame retardant epoxy resin and preparation method thereof
  • A kind of resveratrol-based flame retardant epoxy resin and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 4

[0057] (1) Add 0.008762 mol of resveratrol to a round bottom flask with a condenser tube, and place it under N2 environment. Add 0.07mol epichlorohydrin into the flask at room temperature, heat to 70°C, slowly add 11.683g 30wt% NaOH solution, and keep the reaction mixture at this temperature for 30min. After cooling to room temperature, the product was obtained by filtration, washed three times with xylene, and then vacuum-dried at 30° C. for 8 h to obtain the product RA1.

[0058] (2) Add 0.01 mol of abietic acid to a three-neck flask equipped with mechanical stirring, heating and condensing tubes, raise the temperature to 100°C under nitrogen protection and maintain heating at this temperature for 1 hour, then slowly cool to 100°C, and add 40mL of glacial acetic acid , 0.018mol of maleic anhydride and 0.033g of ferric chloride were reacted under reflux for 3h. Cool to room temperature and filter directly to obtain a light yellow solid, which is recrystallized twice with gla...

Embodiment 5

[0064] (1) Add 0.008762mol resveratrol in the round bottom flask with condenser tube, place N 2 in environment. Add 0.07mol epichlorohydrin into the flask at room temperature, heat to 130°C, slowly add 11.683g 30wt% NaOH solution, and keep the reaction mixture at this temperature for 90min. After cooling to room temperature, the product was obtained by filtration, washed three times with dichloromethane, and then vacuum-dried at 100° C. for 12 h to obtain the product RA1.

[0065] (2) Add 0.019mol RA1 N,N-dimethylformamide solution (180ml) into a round bottom flask with a condenser tube, add 0.0095mol zinc chloride to the solution, stir vigorously, slowly add 0.0228mol Triethyl phosphate, and the reaction mixture was kept at 40°C for 15h. After the reaction, N,N-dimethylformamide was removed. Add 300ml of dichloromethane, wash with saturated ammonium chloride solution and deionized water three times in turn, dry the organic phase with anhydrous sodium sulfate, filter to rem...

Embodiment 6

[0072] (1) Add 0.008762 mol of resveratrol to a round bottom flask with a condenser tube, and place it under N2 environment. 0.07mol epichlorohydrin was added into the flask at room temperature, heated to 100°C, 11.683g 30wt% NaOH solution was slowly added, and the reaction mixture was kept at this temperature for 60min. After cooling to room temperature, the product was obtained by filtration, washed with butanone three times, and then vacuum-dried at 80° C. for 10 h to obtain the product RA1.

[0073] (2) add the tetrahydrofuran solution (100ml) of 0.019mol RA1 in the round-bottomed flask with condensing tube, join 0.0095mol triethylamine in the solution, vigorously stir, slowly add 0.0228mol triethyl phosphite, reaction mixture is in Keep at 30°C for 10h. After the reaction was complete, tetrahydrofuran was removed. Add 200ml butanone to wash twice, the organic phase is dried with anhydrous sodium sulfate, and the sodium sulfate is removed by centrifugation.

[0074] (3)...

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Abstract

The invention provides a resveratrol-based flame-retardant epoxy resin, which uses the hydroxyl group on resveratrol to introduce triethyl phosphite and epoxy groups, and the obtained bio-based epoxy monomer can replace general industrial Bisphenol A (DGEBA) used on Synthesized a bio-based curing agent with high activity—maleopimaric anhydride (MPA), mixed with the prepared epoxy monomer and cured under certain conditions, and prepared a fully bio-based epoxy resin with flame retardant properties . The source of raw materials is wide, green and environmentally friendly, and the synthesis method is relatively simple, and the flame retardancy of epoxy resin is good, the limiting oxygen index can reach up to 52%, and the vertical combustion level can reach up to V‑0 level. The invention discloses its preparation method.

Description

technical field [0001] The invention relates to a resveratrol-based flame-retardant epoxy resin, which introduces phosphorus element into a bio-based epoxy monomer to make it have good flame-retardant performance. Background technique [0002] Due to its various excellent properties, petroleum-based plastics can provide various raw materials and products for various industries such as construction, automobiles, machinery manufacturing, and electronic information, and play a very important role in modern social life. However, in the face of In today's world oil energy crisis and the increasing problem of environmental pollution, people began to look for biomass and renewable resources as raw materials to produce new materials that meet the needs to replace petroleum-based materials. Most biological materials are non-toxic, harmless and rich in content, which can alleviate the pressure of energy depletion and aggravated pollution, reduce the dependence of the plastic industry ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/06C08G59/14C08G59/30C08G59/42
CPCC08G59/063C08G59/1488C08G59/304C08G59/4215
Inventor 丁寅
Owner NANJING UNIV
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