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Monomer of bio-based benzoxazine resin, 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: 2020-04-24
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 bisphenol A is mainly derived from petroleum products , will cause excessive dependence on petroleum products; and bisphenol A will also pollute the environment; in addition, the process of synthesizing benzoxazine resin with existing materials will also cause high polymerization temperature and unsatisfactory curing process.

Method used

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  • Monomer of bio-based benzoxazine resin, benzoxazine resin and preparation method thereof
  • Monomer of bio-based benzoxazine resin, benzoxazine resin and preparation method thereof
  • Monomer of bio-based benzoxazine resin, benzoxazine resin and preparation method thereof

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Embodiment 1

[0044] The preparation method of the low-temperature curing bio-based benzoxazine resin in this embodiment comprises the following steps:

[0045] (1) In a three-necked round-bottomed flask equipped with a magnetic stirrer and a spherical condenser, add 0.01 mol of rhizoid acid, 0.02 mol of furfurylamine, 0.02 mol of polyoxymethylene and 100 ml of dioxane in sequence. After stirring until completely dissolved, the temperature was slowly raised to the reflux state, and the reaction was performed at a constant temperature at the temperature of the reflux state for 8 hours. The clear reaction solution was washed with 200 ml of ethyl acetate water (ethyl acetate:water) solution with a volume ratio of 3:1, and allowed to stand for crystallization. The white powder was obtained by filtration, that is, bio-based rhizoic acid / furfurylamine type benzoxazine resin monomer (PHA-F-Boz), with a yield of 82.7% and a purity of 95.2%.

[0046] (2) Put the product of step (1) into the pre-pre...

Embodiment 2

[0048] The preparation method of the low-temperature curing bio-based benzoxazine resin in this embodiment comprises the following steps:

[0049] (1) In a three-necked round-bottomed flask equipped with a magnetic stirrer and a spherical condenser, add 0.01 mol of rhizoid acid, 0.01 mol of furfurylamine, 0.02 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. Wash the clarified reaction solution with 200ml of 3:1 ethyl acetate aqueous solution, and let it stand for crystallization. The white powder was obtained by filtration, that is, bio-based rhizoic acid / furfurylamine type benzoxazine resin monomer (PHA-F-Boz), with a yield of 72.7% and a purity of 92.2%.

[0050] (2) Put the product of step (1) into the pre-prepared mold and put it in a blast drying oven for segmental curing. The heating process of...

Embodiment 3

[0052] The preparation method of the low-temperature curing bio-based benzoxazine resin in this embodiment comprises the following steps:

[0053] (1) In a three-necked round-bottomed flask equipped with a magnetic stirrer and a spherical condenser, add 0.01 mol of rhizoid acid, 0.02 mol of furfurylamine, 0.02 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 8 hours. Wash and clarify the reaction liquid with 3:1 ethyl acetate aqueous solution 300ml, and let stand to crystallize. The white powder was obtained by filtration, that is, bio-based rhizoic acid / furfurylamine type benzoxazine resin monomer (PHA-F-Boz), with a yield of 93.7% and a purity of 97.2%.

[0054] (2) Put the product of step (1) into the pre-prepared mold and put it in a blast drying oven for segmental curing. The heating process of segmental ...

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Abstract

The invention discloses a monomer of bio-based benzoxazine resin, the benzoxazine resin and a preparation method thereof. The structural formula of the resin is shown as the following formula (II). According to the biomass benzoxazine resin disclosed by the invention, phlorenic acid and furfuryl amine are respectively used as a phenol source and an amine source. PHA molecules have phenolic hydroxyl structures similar to those of phenol, so that PHA serving as a polymer monomer from a bio-based source can completely replace phenol or bisphenol A to be used for preparing high polymer materials such as benzoxazine resin and the like; F is also a common biomass fine chemical raw material produced from plant raw materials such as corncobs, cottonseed hulls, bagasse and the like in nature; by taking phlorenic acid as a phenol source and furfuryl amine as an amine source, excessive dependence of traditional benzoxazine resin on petroleum products is eliminated.

Description

technical field [0001] The invention relates to the technical field of bio-based thermosetting resins and their preparation, in particular to a low-temperature curing (end curing temperature is lower than 200 ° C) and high temperature resistance (under nitrogen conditions, the initial decomposition temperature is 348.5 ° C, respectively, and at 800 ° C) Monomers of bio-based benzoxazine resins with carbon residues as high as 53.1%, respectively, benzoxazine resins prepared from monomers, and preparation methods 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 ...

Claims

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Application Information

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IPC IPC(8): C07D413/06C08G14/06
CPCC07D413/06C08G14/06
Inventor 闫红强詹佐民程捷方征平
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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