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Method for modifying benzoxazine resin

A technology of benzoxazine and resin, which is applied in the field of modified benzoxazine resin, can solve the problems of polluting the environment and not being widely and efficiently used, and achieves the effect of low curing temperature and maintaining excellent performance

Inactive Publication Date: 2011-08-24
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the pulp and paper industry separates cellulose from plants every year, about 50 million tons of waste lignin can be obtained, and more than 95% of the lignin is still directly discharged into rivers or concentrated and burned, and has not been widely and efficiently used. use, and seriously pollute the environment

Method used

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  • Method for modifying benzoxazine resin
  • Method for modifying benzoxazine resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 100g industrial alkali lignin into a 500mL beaker, add 1% dilute sulfuric acid and stir for 30 minutes, then filter, wash the sulfuric acid-treated alkali lignin 3 times with water, the washing liquid is neutral, and the purified alkali lignin obtained at room temperature Let dry. Then put it in a vacuum oven at 60℃ to dry to constant weight, and store in a desiccator.

Embodiment 2

[0026] Add aniline (1mol) and paraformaldehyde (1mol) into a 250mL four-necked flask equipped with a thermometer, agitator, condenser, and dripping device. Stir evenly, then add toluene and raise the temperature to 100°C and stir for 2 hours, then cool down again. Phenol (1mol) or bisphenol A (0.5mol) and paraformaldehyde (1mol) were added, and the temperature was raised to 100°C while stirring to continue stirring for 1 hour. After the reaction is finished, it is filtered and dried after cooling, dissolved with ether, washed with sodium hydroxide solution 3 times, and washed 3 times with water. After drying with magnesium sulfate, the ether is removed with a rotary evaporator to obtain phenol monobenzoxazine monomer (PAF), or double Phenol A type bisbenzoxazine monomer (BAF). NMR analysis results: 1 H-NMR (DMSO, ppm): 4.0 (2H, Ar-CH 2 -N), 4.76(2H, O-CH 2 -N-), 1.0~1.2(3H, -CH 3 ), 3.7(2H, O-CH 2 -). The peak curing temperature measured by DSC is 254°C for PAF and 261°C for B...

Embodiment 3

[0028] Put 120g pyridine into a 500mL three-necked flask, weigh 30g alkali lignin under stirring, and add 70g phenol monobenzoxazine monomer PAF or bisphenol A dibenzoxazine monomer BAF after the lignin is dissolved, continue Stir for 30 minutes, pour out the mixture in a petri dish, put it in a vacuum oven to dry, a part of the solid obtained is used for DSC to test the curing start temperature T onset And peak temperature T p , The other part is cured in an electric oven according to the process of 120℃ / 2h+140℃ / 2h+160℃ / 6h and then used TGA to test the maximum thermal weight loss rate temperature T of the polybenzoxazine resin max And 800℃ residual carbon rate. The specific results are listed in Table 1.

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Abstract

The invention discloses a method for modifying a benzoxazine resin, which comprises the following steps: adding natural lignin into benzoxazine monomer, and curing after the crosslinking temperature of the benzoxazine is reduced to 50 DEG C. The thermal weightlessness temperature of the lignin-cured benzoxazine resin is increased, and the carbon residue rate is up to more than 40%. The lignin can be used as a catalyst, and can also be used as a filler for improving the properties of the benzoxazine resin, thereby increasing the reutilization ratio of the lignin and reducing the problem in the curing of the benzoxazine resin.

Description

Technical field [0001] The invention relates to a method for modifying a benzoxazine resin. After the by-product natural alkaline lignin and benzoxazine monomers are mixed uniformly, the curing temperature of the benzoxazine resin is reduced and the curing temperature of the benzoxazine resin is reduced to improve The processing properties of benzoxazine. It belongs to the fields of forestry chemistry, polymer materials science and engineering technology. Background technique [0002] Benzoxazine is a six-membered heterocyclic compound synthesized by Mannich reaction of phenolic compounds, amine compounds and formaldehyde as raw materials. Benzoxazine can be ring-opened and polymerized to form polybenzoxazine materials. The structure of polybenzoxazine material is similar to that of phenolic resin and has the characteristics of phenolic resin, but it overcomes the shortcomings of traditional Novolac-type phenolic resin and Resole-type phenolic resin. Polybenzoxazine materials ...

Claims

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Application Information

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IPC IPC(8): C08G73/06C08H7/00C08L79/04
Inventor 黄发荣诺爱丁袁荞龙
Owner EAST CHINA UNIV OF SCI & TECH
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