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Tannin type benzoxazine and preparation method thereof

A benzoxazine and tannin-type technology, applied in the field of tannin-type benzoxazine and its preparation, can solve problems such as unmanned research, achieve the effects of promoting ring-opening polymerization, reducing curing temperature, and broadening the preparation route

Active Publication Date: 2021-02-02
GUANGXI TEACHERS EDUCATION UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the introduction of tannins into benzoxazines as a phenol source has not yet been studied.

Method used

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  • Tannin type benzoxazine and preparation method thereof
  • Tannin type benzoxazine and preparation method thereof
  • Tannin type benzoxazine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: Preparation of tannin-phenol-furfurylamine type benzoxazine

[0034] First, add paraformaldehyde and distilled water into a three-neck flask equipped with a condenser tube and a stirring device, heat and stir to dissolve them all to obtain an aqueous formaldehyde solution. After cooling to room temperature, add furfurylamine and xylene, react at room temperature for 30 minutes, add phenol, xylene and ethanol mixed solution, raise the temperature of the above mixed system to 80°C, add tannin solution after reacting for 1 hour, and heat at 80°C The reaction was continued for 2.5 hours to obtain a mixture of tannin-phenol-furfurylamine benzoxazine, and the resulting mixture was washed with ethanol and warm water to neutrality, and then the solvent was removed by a rotary evaporator, and then placed in a vacuum drying in an oven at 75°C for 1 hour to obtain a brown solid resin, which is a tannin-phenol-furfurylamine type benzoxazine, and the greater the tannin...

Embodiment 2

[0035] Embodiment 2: Preparation of tannin-hydroquinone-cyclohexylamine type benzoxazine

[0036] First, add paraformaldehyde and distilled water into a three-neck flask equipped with a condenser tube and a stirring device, heat and stir to dissolve them all to obtain an aqueous formaldehyde solution. After cooling to room temperature, add cyclohexylamine and dioxane, react in ice bath for 30 minutes, then add hydroquinone, raise the temperature of the above mixed system to 80°C, add tannin solution and dioxane after 1 hour of reaction Mix the solution with ethanol, and continue to react at 80°C for 2.5 hours to obtain a mixture of tannin-hydroquinone-cyclohexylamine-type benzoxazine, wash the resulting mixture with ethanol and warm water to neutrality, and pass through The solvent was removed by a rotary evaporator, then placed in a vacuum oven, and dried at 75°C for 1 hour to obtain a brown solid resin, which was a tannin-hydroquinone-cyclohexylamine type benzoxazine, and th...

Embodiment 3

[0037] Embodiment 3: preparation tannin-phenol-aniline type benzoxazine (T-Pa)

[0038]First, add paraformaldehyde and distilled water into a three-neck flask equipped with a condenser tube and a stirring device, heat and stir to dissolve them all to obtain an aqueous formaldehyde solution. After cooling to room temperature, add aniline and toluene, react at room temperature for 30 minutes, add phenol, toluene and ethanol mixed solution, raise the temperature of the above mixed system to 80°C, add tannin solution after reacting for 1 hour, and continue the reaction at 80°C After 2.5 hours, the tannin-phenol-aniline benzoxazine mixture was obtained, and the resulting mixture was washed with ethanol and warm water to neutrality, and then the solvent was removed by a rotary evaporator, and then placed in a vacuum oven, and Dry at 75°C for 1 hour to obtain a brown solid resin, which is tannin-phenol-aniline benzoxazine (T-Pa). The greater the tannin content, the darker the resin c...

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PUM

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Abstract

The invention discloses a preparation method of tannin type benzoxazine, comprising: step 1, dissolving paraformaldehyde in solvent 1, adding amines and solvent 2, after reaction, adding phenolic mixture and solvent 3, heating, Continue the reaction to obtain a tannin-type benzoxazine mixture; step 2, wash the tannin-type benzoxazine mixture to neutrality, and remove the solvent to obtain a tannin-type benzoxazine; wherein, the The phenolic mixture includes tannins. The invention synthesizes the benzoxazine by replacing part of the phenol source with tannin, lowers the ring-opening polymerization temperature of the prepared tannin-type benzoxazine, and maintains the excellent thermal performance of the traditional benzoxazine.

Description

technical field [0001] The invention relates to the field of preparation of benzoxazines. More specifically, the present invention relates to a tannin-type benzoxazine and a preparation method thereof. Background technique [0002] Benzoxazine is a new type of phenolic resin, which can undergo ring-opening polymerization reaction under the action of heating and (or) catalyst to form a cross-linked structure similar to phenolic resin. Benzoxazine not only has the good thermal and electrical properties of traditional phenolic resins, but also has the advantages of not requiring strong acid or strong base as a catalyst during curing, no small molecule release during curing, and close to zero shrinkage in volume. Therefore, in recent years, benzoxazines have received extensive attention and obtained industrial applications. However, benzoxazine also has some disadvantages, such as high brittleness and high ring-opening polymerization temperature, etc., which limit its applicat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G14/06
CPCC08G14/06
Inventor 朱永飞王乐萌程马力苏俊铭李沛林
Owner GUANGXI TEACHERS EDUCATION UNIV