Low-temperature curable bio-based benzoxazine resin and preparation method thereof

A technology of oxazine resin and benzoxazine, which is applied in the field of bio-based thermosetting resin and its preparation, can solve the problems of unsatisfactory curing process, dependence on petroleum products, high polymerization temperature, etc., and achieve low cost, high yield and high purity Effect

Active Publication Date: 2019-08-16
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, the main source of phenol for the synthesis of benzoxazine resins is bisphenol A (Bisphenol A, BPA), but the main source of bisphenol A is petroleum products, causing excessive dependence on petroleum product

Method used

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  • Low-temperature curable bio-based benzoxazine resin and preparation method thereof
  • Low-temperature curable bio-based benzoxazine resin and preparation method thereof
  • Low-temperature curable bio-based benzoxazine resin and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0037] The preparation method of the low-temperature curing bio-based benzoxazine resin in this embodiment comprises the following steps:

[0038] (1) In a three-neck round bottom flask equipped with a magnetic stirrer and a spherical condenser, add 0.04 mol of furfurylamine, 0.01 mol of phloroglucinol, 0.06 mol of polyoxymethylene and 100 ml of dioxane in sequence. After stirring until completely dissolved, the temperature was slowly raised to a reflux state, and the reaction was carried out at a constant temperature for 8 hours. The clear reaction solution was washed with petroleum ether to obtain a colorless and transparent solution. The obtained solution was rotatively evaporated to obtain a white powder, namely bio-based phloroglucinol furfurylamine type benzoxazine resin monomer (PHG-F), with a yield of 82.7% and a purity of 98.2%.

[0039] (2) In a three-neck round bottom flask equipped with a magnetic stirrer and a spherical condenser, add 0.04mol of p-aminobenzoic ac...

Embodiment 2

[0042] The preparation method of the low-temperature curing bio-based benzoxazine resin in this embodiment comprises the following steps:

[0043] (1) In a three-neck round bottom flask equipped with a magnetic stirrer and a spherical condenser, add 0.03 mol of furfurylamine, 0.01 mol of phloroglucinol, 0.06 mol of polyoxymethylene and 100 ml of dioxane in sequence. After stirring until completely dissolved, the temperature was slowly raised to a reflux state, and the reaction was carried out at a constant temperature for 6 hours. The clear reaction solution was washed with petroleum ether to obtain a colorless and transparent solution. The obtained solution was rotatively evaporated to obtain a white powder, namely bio-based phloroglucinol furfurylamine type benzoxazine resin monomer (PHG-F), with a yield of 51.6% and a purity of 97.8%.

[0044] (2) In a three-neck round bottom flask equipped with a magnetic stirrer and a spherical condenser, add 0.03 mol of p-aminobenzoic a...

Embodiment 3

[0047] The preparation method of the low-temperature curing bio-based benzoxazine resin in this embodiment comprises the following steps:

[0048] (1) In a three-neck round bottom flask equipped with a magnetic stirrer and a spherical condenser, add 0.04 mol of furfurylamine, 0.01 mol of phloroglucinol, 0.08 mol of polyoxymethylene and 150 ml of dioxane in sequence. After stirring until completely dissolved, the temperature was slowly raised to a reflux state, and the reaction was carried out at a constant temperature for 10 hours. The clear reaction solution was washed with petroleum ether to obtain a colorless and transparent solution. The obtained solution was rotatively evaporated to obtain a white powder, namely bio-based phloroglucinol furfurylamine type benzoxazine resin monomer (PHG-F), with a yield of 93.2% and a purity of 99.1%.

[0049] (2) In a three-neck round bottom flask equipped with a magnetic stirrer and a spherical condenser, add 0.04 mol of p-aminobenzoic ...

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Abstract

The invention discloses low-temperature curable bio-based benzoxazine resin and a preparation method thereof. The benzoxazine resin monomer is prepared from bio-based m-trihydroxybenzene, furfuryl amine and paraformaldehyde; and under the catalytic condition of a catalyst prepared from bio-based m-trihydroxybenzene, p-aminobenzoic acid and paraformaldehyde, the low-temperature curing characteristic of curing completely at 200 DEG C is realized. The product is suitable for preparation of a natural fiber-reinforced green composite material. The synthetic process of the monomer and the catalyst is reasonable, purity is high, raw materials are bio-based raw materials and green and environmentally-friendly, yield is high, and the cost is economical and reasonable. The structural formula of theproduct is as shown in the formula (I).

Description

technical field [0001] The present invention relates to a bio-based thermosetting resin and the technical field of preparation thereof, in particular to a bio-based benzoxazine resin cured at low temperature (140°C as the initial curing temperature and 190°C as the end curing temperature) and a preparation method thereof . Background technique [0002] Polymer materials are the most rapidly developed materials in the twentieth century, but almost all polymers are produced from fossil mineral resources. With the rapid development of the economy, non-renewable resources such as petroleum have become less and less, and it has become an important task for us to find new renewable resources and obtain energy and chemicals from renewable resources. [0003] The benzoxazine resin is prepared by reacting phenolic compounds, primary amine compounds and formaldehyde to form monomers, and then cross-linking and curing under the action of heating and / or catalysts. Compared with tradit...

Claims

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Application Information

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IPC IPC(8): C08G14/073
CPCC08G14/06
Inventor 闫红强詹佐民程捷方征平
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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