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Monomer of benzoxazine resin, benzoxazine resin and preparation method of benzoxazine resin

A benzoxazine and resin technology, 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 curing temperature, and achieve the effects of low cost, high yield and high purity

Active Publication Date: 2020-05-12
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, bisphenol A (Bisphenol A, BPA) is the main source of phenol for the synthesis of benzoxazine resins, 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 curing temperature and unsatisfactory curing process

Method used

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  • Monomer of benzoxazine resin, benzoxazine resin and preparation method of benzoxazine resin
  • Monomer of benzoxazine resin, benzoxazine resin and preparation method of benzoxazine resin
  • Monomer of benzoxazine resin, benzoxazine resin and preparation method of benzoxazine resin

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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-neck round bottom flask equipped with a magnetic stirrer and a spherical condenser, add 0.01mol of p-coumaric acid, 0.02mol of furfurylamine, 0.02mol of polyoxymethylene and 100ml of dioxane in sequence, and stir until completely dissolved The temperature was slowly raised to a reflux state, and kept at the temperature of the reflux state for a constant temperature reaction for 8 hours. The obtained turbid solution was filtered to obtain a clear solution, cooled and crystallized in an ice-water bath to obtain a white powder, namely bio-based p-coumaric acid / furfurylamine type benzoxazine monomer (PRA-F-Boz), with a yield of 85.0% and a purity of 94.8% .

[0046] (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 curing is...

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-neck round bottom flask equipped with a magnetic stirrer and a spherical condenser, add 0.01mol of p-coumaric acid, 0.01mol of furfurylamine, 0.02mol of polyoxymethylene and 100ml of dioxane in sequence, and stir 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 resulting turbid solution was filtered to obtain a clear solution, cooled and crystallized in an ice-water bath to obtain a white powder, namely bio-based p-coumaric acid / furfurylamine benzoxazine monomer (PRA-F-Boz), with a yield of 75.0% and a purity of 91.8% .

[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 segmental curing is: 180°C / 1h, 185°C / 2h, 190°C / 1...

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-neck round bottom flask equipped with a magnetic stirrer and a spherical condenser, add 0.01mol of p-coumaric acid, 0.02mol of furfurylamine, 0.02mol of polyoxymethylene and 150ml of dioxane in sequence, and stir 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 resulting turbid solution was filtered to obtain a clear solution, cooled and crystallized in an ice-water bath to obtain a white powder, namely bio-based p-coumaric acid / furfurylamine type benzoxazine monomer (PRA-F-Boz), with a yield of 94.0% and a purity of 97.8% .

[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 curing is: 180°C / 1h, 185°C / 2h, 19...

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Abstract

The invention relates to a monomer of a benzoxazine resin, a benzoxazine resin and a preparation method of the benzoxazine resin, wherein the structural formula of the benzoxazine resin is representedby the following formula (II). According to the benzoxazine resin disclosed by the invention, p-coumaric acid and furfuryl amine are respectively used as a phenol source and an amine source, And PRAmolecules have phenolic hydroxyl structures similar to those of phenol, so that PRA serving as a bio-based polymer monomer can completely replace phenol or bisphenol A to be used for preparing high polymer materials such as a benzoxazine resin and the like; FA is also a common biomass fine chemical industry raw material produced from plant raw materials such as corncobs, cottonseed hulls, bagasseand the like in nature; and by taking p-coumaric acid as a phenol source and furfuryl amine as an amine source, excessive dependence of the 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 (the initial decomposition temperature is 347.4°C under nitrogen conditions, and at 800°C The carbon residue is as high as 56.0%) the monomer of the benzoxazine resin, the benzoxazine resin prepared from the monomer and the 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D413/06C08G14/073
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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