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Preparation process of boron-containing bene oxazine resin

A benzoxazine and resin technology, applied in the field of boron-containing benzoxazine resin and its preparation, can solve the problems of large void ratio of products, poor molding processability, poor solubility and the like

Active Publication Date: 2010-01-13
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high curing temperature and poor solubility in ordinary organic solvents of pure boron-modified aldehyde resins, hexamethylenetetramine or other amines are used as curing catalysts, and a large number of small molecules are still released during curing. Defects such as large void ratio, resulting in poor molding process and unstable performance, which limit its development

Method used

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  • Preparation process of boron-containing bene oxazine resin
  • Preparation process of boron-containing bene oxazine resin
  • Preparation process of boron-containing bene oxazine resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Example 1: Add 20 parts of boric acid and 80 parts of phenol into the reaction kettle, heat up (not exceeding 160° C.) for dehydration, and cool down when the desorbed water reaches a certain amount, then add 160 parts of formaldehyde aqueous solution, and use an alkaline catalyst Adjust the pH value of the system to 6-10, add toluene and 40 parts of ethylenediamine to carry out temperature rise and reflux reaction for 2 hours, then vacuum dehydrate at 80-140°C to obtain boron-containing benzoxazine resin, add solvent to obtain uniform and clear Transparent brown-yellow stable solution of boron-containing benzoxazine resin. The resin solution can be added with an accelerator according to different purposes to adjust the molding time to 5-18min / 160°C.

Embodiment 2

[0062] Example 2: Add 70 parts of boric acid and 240 parts of phenol into the reaction kettle, heat up (not exceeding 160°C) for dehydration, cool down and cool down when the detached water reaches a certain amount, then add 360 parts of formaldehyde aqueous solution, adjust with alkaline catalyst The pH value of the system is 6-10, add toluene, 120 parts of 4,4'diaminodiphenylmethane (MDA) to carry out temperature rise and reflux reaction for 4 hours, then vacuum dehydrate at 80-140°C to obtain boron-containing benzoxazine The resin is added with a solvent to obtain a stable solution of a uniform, clear, transparent brown-yellow boron-containing benzoxazine resin. The resin solution can be added with an accelerator according to different purposes to adjust the molding time to 5-18min / 160°C.

Embodiment 3

[0063] Example 3: Add 70 parts of boric acid and 240 parts of phenol into the reaction kettle, heat up (not exceeding 160°C) for dehydration, cool down when the desorbed water reaches a certain amount, then add toluene and 160 parts of formaldehyde aqueous solution, and use an acidic catalyst Adjust the pH value of the system to 1-3, heat up and reflux for 2 hours and then lower the temperature, adjust the pH value of the system to 6-10 with an alkaline catalyst, add 120 parts of aniline, 200 parts of formaldehyde aqueous solution and a small amount of toluene and alcohol, and heat up at 80 After reflux reaction at ~90°C for 2 hours, vacuum dehydration at 80-120°C to obtain a boron-containing benzoxazine resin, adding a solvent to obtain a uniform, clear, transparent brown-red stable solution of the boron-containing benzoxazine resin. The resin solution can be added with an accelerator according to different purposes to adjust the molding time to 5-18min / 160°C.

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Abstract

The process of preparing boron-containing benzoxazine resin includes the following steps: 1. preparing materials including boric acid 20-70 weight portions, phenolic compound 80-240 weight portions, amine compound 40-120 weight portions, water solution of formaldehyde 160-360 weight portions, acid catalyst 1-4 weight portions and alkaline catalyst 4-8 weight portions; and 2. reaction of boric acid, phenolic compound and acid catalyst in a reactor, and heated reflux dewatering to obtain borate; heating to 50 deg.c, adding partial formaldehyde to synthesize boron-containing linear phenolic resin; adding alkaline catalyst to regulate pH to 6-9, adding amine compound and the rest formaldehyde to reflux react at 85-95 deg.c for 2-8 hr, and vacuum dewatering or reflux dewatering at 80-140 deg.c to obtain the boron-containing benzoxazine resin. The resin is used in producing electrically insulating material and product in high flame retarding level.

Description

technical field [0001] The invention belongs to the field of thermosetting resin synthesis, and relates to a boron-containing benzoxazine resin and its preparation method and application. Background technique [0002] In the 1940s, foreign countries conducted systematic research on the reaction of phenolic compounds, amine compounds and formaldehyde, and synthesized compounds containing Benzoxazine (Benzoxazine) ring structure. Compared with other condensation reactions related to phenolic formaldehyde, the outstanding feature of this reaction is that the phenolic hydroxyl group participates in the ring-closing reaction. [0003] [0004] R = hydrogen, halogen atom, alkyl, alkoxy, etc. [0005] R' = aliphatic or aromatic group [0006] Since the 1970s, foreign countries have carried out preliminary research on the ring-opening polymerization reaction and product development of benzoxazine. Since the 1990s, extensive research has been carried out at home and abroad on t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C09J179/04B32B37/12
Inventor 刘锋唐安斌马庆柯许自贵李仕文
Owner SICHUAN DONGFANG INSULATING MATERIAL
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