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Method for preparing bio-based flame-retardant epoxy resin and prepared bio-based flame-retardant epoxy resin

A technology of epoxy resin and preparation method, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of non-renewability, poor flame retardancy, and toxic raw materials, and achieve improvement Cross-linking density, improved thermal stability, simple and low toxicity in the reaction process

Active Publication Date: 2018-06-22
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 solve the problem that traditional synthetic resins have poor flame retardancy and raw materials are toxic and non-renewable, and provide a method for preparing a fully bio-based flame-retardant epoxy resin

Method used

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  • Method for preparing bio-based flame-retardant epoxy resin and prepared bio-based flame-retardant epoxy resin
  • Method for preparing bio-based flame-retardant epoxy resin and prepared bio-based flame-retardant epoxy resin
  • Method for preparing bio-based flame-retardant epoxy resin and prepared bio-based flame-retardant epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Put 20ml tetrahydrofuran, 0.088mol potassium carbonate, and 0.0176mol gallic acid into a sealed flask, and vigorously stir for 5 minutes. Then, a solution of allyl bromide was slowly added over 20 min. The mixture was heated to 50 °C and maintained at this temperature for 20 h. The obtained product was filtered to remove impurities in the solution, and then rotary evaporated. Finally, the crude product was dissolved in dichloromethane and washed with saturated brine. The dichloromethane layer was evaporated by rotary evaporation to obtain the refined product, which was dried under vacuum at 50°C for 7 hours to obtain the product 1.

[0030](2) Add 0.0176mol DOPO and 30ml tetrahydrofuran into a round bottom flask with a condenser, and heat to 60°C under an argon atmosphere. After complete dissolution of DOPO, 0.0176 mol of product 1 was added within 30 min and the reaction mixture was kept at this temperature for 10 h. After cooling to room temperature, the produ...

Embodiment 2

[0038] (1) Put 20ml of dichloromethane, 0.088mol of potassium carbonate and 0.0176mol of gallic acid into a sealed flask, and vigorously stir for 20min. Then, a solution of allyl bromide in dichloromethane was slowly added over 60 min. The mixture was heated to 80 °C and maintained at this temperature for 48 h. The resulting product was filtered and rotary evaporated. Finally, the crude product was dissolved in dichloromethane and washed with saturated brine. The dichloromethane layer was evaporated by rotary evaporation to obtain the refined product, and the product 1 was obtained by vacuum drying at 80° C. for 15 h.

[0039] (2) Add 0.0176 mol of DOPO and 80 ml of dichloromethane into a round bottom flask with a condenser, and heat the flask to 100° C. under an argon atmosphere. After complete dissolution of DOPO, 0.0176 mol of product 1 was added within 80 min, and the reaction mixture was kept at this temperature for 40 h. After cooling to room temperature, the product...

Embodiment 3

[0047] (1) Put 30ml of acetone, 0.088mol of potassium carbonate and 0.0176mol of gallic acid into a sealed flask, and stir vigorously for 15min. Then, a solution of allyl bromide in acetone was slowly added within 40 min. The mixture was heated to 60 °C and maintained at this temperature for 30 h. The resulting product was filtered and rotary evaporated. Finally, the crude product was dissolved in dichloromethane and washed with saturated brine. The dichloromethane layer was evaporated by rotary evaporation to obtain the refined product, and the product 1 was obtained by vacuum drying at 70° C. for 10 h.

[0048] (2) Add 0.0176mol DOPO and 50ml acetone to a round bottom flask with a condenser, and heat the flask to 80°C under an argon atmosphere. After complete dissolution of DOPO, 0.0176 mol of product 1 was added within 50 min, and the reaction mixture was kept at this temperature for 30 h. After cooling to room temperature, the product was obtained by filtration, washed...

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Abstract

The invention discloses a total-bio-based flame-retardant epoxy resin. According to the invention, reactive groups on gallic acid are used for introducing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and epoxy groups so as to obtain a bio-based epoxy monomer which is used for replacing bisphenol A epoxy resin DGEBA used in general industries; and a bio-based curing agent, i.e., difurfurylamine, with higher activity is synthesized and subjected to mixing and curing with the prepared epoxy monomer so as to prepare a total-bio-based epoxy resin product with flame retardant properties. The epoxy resin is rich in biological sources, friendly to environment, simple in reaction process and good in flame retardancy, and has a highest limit oxygen index of 34% and a highest vertical burning level of V-0. The invention also discloses a preparation method for the total-bio-based flame-retardant epoxy resin.

Description

technical field [0001] The invention relates to a fully bio-based flame-retardant epoxy resin. Phosphorus is introduced into the 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 on the supp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/30C08G59/26C08G59/38C08G59/50C07F9/6574
CPCC07F9/657172C08G59/26C08G59/304C08G59/38C08G59/504C08G59/5046
Inventor 丁寅潘政
Owner NANJING UNIV
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