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Low temperature curing 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 the goal of getting rid of excessive dependence, low cost and high purity Effect

Active Publication Date: 2021-10-22
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 products; and bisphenol A Also can cause pollution to environment; In addition, existing material synthesis benzoxazine resin process also can cause polymerization temperature high, the deficiency of unsatisfactory curing process

Method used

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

Examples

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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 a low-temperature curing bio-based benzoxazine resin and a preparation method thereof. The benzoxazine resin monomer is prepared from bio-based sources of phloroglucinol, furfurylamine and paraformaldehyde, and prepared from bio-based sources of phloroglucinol, p-aminobenzoic acid and paraformaldehyde Under the catalytic conditions of the catalyst, the low-temperature curing characteristics of complete curing at 200 ° C are realized, which is suitable for the preparation of natural fiber-reinforced green composite materials. The synthesis process of the monomer and the catalyst is reasonable, the purity is high, the raw material is a biomass raw material, green and environmentally friendly, the yield is high and the cost is reasonable, and its structural formula is shown in the following 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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Patent Type & Authority Patents(China)
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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