A kind of preparation method and application of whole biological source benzoxazine resin

A benzoxazine and all-biological technology is applied in the field of preparation of all-biological source benzoxazine resin, which can solve the problems of long reaction time and high curing temperature, and achieve narrow molecular weight distribution, high reaction efficiency and uniform product structure. Effect

Active Publication Date: 2021-11-12
淮北绿洲新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of benzoxazine based on bisphenolic acid and furfurylamine has been reported, but the existing preparation method is carried out in a non-polar solvent, the reaction time is long (10-15h), and the curing temperature is high (230-250°C) (CN201810013847 -biomass bisphenolic acid-furfurylamine type benzoxazine resin and its preparation method)

Method used

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  • A kind of preparation method and application of whole biological source benzoxazine resin
  • A kind of preparation method and application of whole biological source benzoxazine resin
  • A kind of preparation method and application of whole biological source benzoxazine resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Preparation of benzoxazine prepolymers from all biological sources:

[0045] In a nitrogen atmosphere, under the condition of no solvent, add 5.82g (0.06mol) furfurylamine and 3.60g (0.12mol) paraformaldehyde into a 250mL three-necked flask equipped with a condenser, magnetic stirring, and thermometer, mix well and heat React at 160°C for 0.25h, then add 8.58g (0.03mol) of natural bisphenolic acid, mix well and react at 160°C for 0.75h, the molar ratio of aldehyde, phenolic hydroxyl and amino functional groups is 2:1:1, after the reaction Pour the reaction solution into methanol solution (concentration 85wt%) and let it stand for 24 hours. After standing, remove the supernatant to obtain a yellow powder. Dry the yellow powder under vacuum at 60°C for 8 hours. The final dried product is the whole biological source benzo Oxazine prepolymers. The yield was 99.5%, and the molecular weight distribution was 1.16.

Embodiment 2

[0047] Preparation of benzoxazine prepolymers from all biological sources:

[0048] In a nitrogen atmosphere and without solvent, add 4.85g (0.05mol) furfurylamine and 3.00g (0.10mol) paraformaldehyde into a 250mL three-necked flask equipped with a condenser, magnetic stirring, and thermometer, mix well and heat React at 115°C for 1 hour, then add 8.58g (0.03mol) of natural bisphenolic acid, mix well and react at 115°C for 3 hours. Pour the solution into methanol solution (concentration 50wt%) and let it stand for 24 hours. After standing, remove the supernatant to obtain a yellow powder. Dry the yellow powder under vacuum at 60°C for 8 hours. The final dried product is benzoxazine from all biological sources. prepolymer. The yield was 99.2%, and the molecular weight distribution was 1.12.

Embodiment 3

[0050] Preparation of benzoxazine prepolymers from all biological sources:

[0051] In a nitrogen atmosphere, under the condition of no solvent, add 3.88g (0.04mol) furfurylamine and 2.4g (0.08mol) paraformaldehyde into a 250mL three-necked flask equipped with a condenser, magnetic stirring, and thermometer, mix well and heat React at 140°C for 0.75h, then add 8.58g (0.03mol) of natural bisphenolic acid, mix well and react at 140°C for 2h, the molar ratio of aldehyde group, phenolic hydroxyl group and amino functional group is 1.33:1:0.67, after the reaction Pour the reaction solution into methanol solution (concentration 95wt%) and let it stand for 24 hours. After standing, remove the supernatant to obtain a yellow powder. Dry the yellow powder under vacuum at 60°C for 8 hours. The final dried product is the whole biological source of benzoxan oxazine prepolymers. The yield was 99.6%, and the molecular weight distribution was 1.14.

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Abstract

The invention relates to a preparation method and application of all biological source polybenzoxazine. The whole biological source benzoxazine prepolymer provided by the invention has the advantages of simple process, high reaction efficiency, high product purity, narrow molecular weight distribution, uniform structure of cured product and complete network structure. The all-biological source benzoxazine cured resin obtained by the final temperature-programmed curing of the prepolymer has excellent heat resistance, mechanical properties, flame retardancy and dielectric properties, especially excellent high-frequency dielectric properties, and can be used in High-frequency and high-speed circuit board substrates, microwave and millimeter wave communications, automotive radar and other fields. And because the cured resin has a well-developed cross-linking network and high nitrogen content, the carbonized all-biological source benzoxazine porous resin material can be used as a functional material, and can be applied to electricity storage, drug loading, pollutants, etc. processing, gas adsorption, etc.

Description

technical field [0001] The invention relates to the technical field of organic polymer materials, in particular to a preparation method and application of an all-biological source benzoxazine resin. Background technique [0002] Benzoxazine is a new type of phenolic resin, which is a six-membered heterocyclic compound synthesized from phenolic compounds, amine compounds and aldehydes through Mannich reaction. While maintaining the excellent thermal properties, flame retardancy and electrical insulation of traditional phenolic resins, it also has many advantages that traditional phenolic resins do not have, such as no release of small molecules during processing and curing, and the product has low porosity. , the volume is close to zero shrinkage, the material has better high temperature thermal stability, flame retardancy, mechanical properties and chemical stability, etc., and has low water absorption and no strong acid or strong base catalysis in the preparation process, w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G14/06C08L61/34C08K3/22
CPCC08G14/06C08K3/22C08K2003/2227C08K2003/2241C08K2003/2244C08K2003/2275C08K2003/2296C08K2201/011C08L61/34
Inventor 曾鸣冯子健
Owner 淮北绿洲新材料有限责任公司
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