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Preparation method of complete biogenetic derivation benzoxazine resin and application thereof

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

Active Publication Date: 2019-01-11
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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  • Preparation method of complete biogenetic derivation benzoxazine resin and application thereof
  • Preparation method of complete biogenetic derivation benzoxazine resin and application thereof
  • Preparation method of complete biogenetic derivation benzoxazine resin and application thereof

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 of complete biogenetic derivation benzoxazine resin and application thereof. A complete biogenetic derivation benzoxazine prepolymer is simple in process,high in reaction efficiency, high in product purity, narrow in molecular weight distribution, uniform in solidified product structure and complete in network structure. The complete biogenetic derivation benzoxazine resin obtained by the final procedure, heating for solidification, of the prepolymer has excellent heat resistant property, mechanical property, flame retardant property and dielectric property, has excellent high frequency dielectric property, and can be applied to the fields of high frequency and high speed circuit board base materials, microwave and millimeter wave communication, vehicle-borne radar and the like. While because the solidified resin has developed cross-linked network, and relatively high nitrogen content, and the carbonized complete biogenetic derivation benzoxazine resin can be applied as a functional material, and can be applied to the aspects of electricity storage, drug loading, pollutant treatment, gas adsorption and the like.

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 Applications(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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