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Benzoxazine resin based on apigenin biology base and preparation method thereof

A technology of oxazine resin and apigenin, applied in the field of apigenin-based bio-based benzoxazine resin and preparation thereof, can solve problems such as difficulty in forming a dense cross-linked network structure, poor thermal stability, and increased processing difficulty , to achieve the effect of being suitable for large-scale production, improving cross-linking density, and low equipment requirements

Inactive Publication Date: 2020-04-03
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, compared with traditional benzoxazine resins, the currently developed bio-based benzoxazines also have certain defects.
Monofunctional bio-based benzoxazine resins have poor thermal stability due to difficulty in forming a dense cross-linked network structure after ring-opening curing
In addition, the curing temperature of bio-based benzoxazine is generally high, which increases its processing difficulty

Method used

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  • Benzoxazine resin based on apigenin biology base and preparation method thereof
  • Benzoxazine resin based on apigenin biology base and preparation method thereof
  • Benzoxazine resin based on apigenin biology base and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Use 2-furylmethylamine as the amine source; add 2.70g (0.01mol) of apigenin, 1.94g (0.02mol) of 2-furylmethylamine, 1.32g (0.044mol) of paraformaldehyde into the flask, and then add 50mL of toluene solution , connected to a condenser, stirred at 110°C and reacted for 8 hours; after the reaction was stopped, the reaction solution was washed with water, and the organic solvent was removed by rotary evaporation, and dried in a vacuum oven at 50°C for one day to obtain 4.30g of benzoxazine monomer. Yield 84%. The chemical reaction equation is as follows:

[0032]

[0033] In the present embodiment, the obtained oxazine product structure is:

[0034]

[0035] The product's proton nuclear magnetic resonance spectrum, Fourier transform infrared transform spectrum, DSC curve and thermogravimetric curve are as follows figure 1 , figure 2 , image 3 with Figure 4 shown.

[0036] figure 1 It is a hydrogen nuclear magnetic resonance spectrum, and it can be seen from ...

Embodiment 2

[0041] The amine source compound 2-furylmethylamine in Example 1 was replaced by aniline. Other steps are the same as those in Example 1.

[0042] Wherein the specific chemical structural formula of aniline is: The amount of reactants was changed to: weigh 2.70 g (0.01 mol) of apigenin, 1.86 g (0.02 mol) of aniline, and 1.32 g (0.044 mol) of paraformaldehyde, with a yield of 88%.

[0043]

[0044] The curing exothermic peak temperature of the latent curing type benzoxazine resin monomer obtained in this example is 168°C. After further curing and crosslinking, the temperature of the polybenzoxazine resin is 372°C when the thermal weight loss is 5%. At 800°C, the carbon residue rate is 65%.

Embodiment 3

[0046] The amine source compound 2-furylmethylamine in Example 1 was replaced by m-cyanoaniline. Other steps are the same as those in Example 1.

[0047] The specific chemical structural formula of the middle-cyanoaniline is The amount of reactants was changed to: weigh 2.70 g (0.01 mol) of apigenin, 2.36 g (0.02 mol) of m-cyanoaniline, and 1.32 g (0.044 mol) of paraformaldehyde. Yield 80%.

[0048]

[0049] The curing exothermic peak temperature of the latent curing type benzoxazine resin monomer obtained in this example is 195°C. After further curing and crosslinking, the temperature of the polybenzoxazine resin is 386°C when the thermal weight loss is 5%. At 800°C, the carbon residue rate is 66%.

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Abstract

The invention belongs to the technical field of thermosetting resin. The invention relates to benzoxazine resin based on apigenin biology base and a preparation method thereof, especially to benzoxazine containing a phenolic hydroxyl group and carbon-carbon double bonds at the same time and preparation method thereof. The preparation method comprises the steps of: mixing apigenin, an amine compound and paraformaldehyde, adding the obtained mixture into a low-polarity solvent for reaction for 6-18 h at a temperature of 80-120 DEG C, washing the mixture with water after the reaction, performingrotary evaporation to remove an organic solvent, and drying the mixture to obtain the product. The benzoxazine resin based on apigenin biology base and the preparation method thereof have the advantages that apigenin is used as a phenol source of the benzoxazine resin, and the synthesized benzoxazine resin contains phenolic hydroxyl, so that the curing temperature can be reduced; the carbon-carbondouble bonds provided by apigenin can be used for further improving the crosslinking density of the benzoxazine resin through crosslinking reaction; and moreover, the synthesis steps are simple, theyield is high, the cured benzoxazine resin has very excellent thermal and mechanical properties, the synthesis process is easy to implement, and the benzoxazine resin is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of thermosetting resins, in particular to an apigenin-based bio-based benzoxazine resin and a preparation method thereof. Background technique [0002] Benzoxazine resin is a new type of thermosetting material synthesized from phenol source, amine source and formaldehyde. Compared with traditional thermosetting resins, benzoxazine resins have attracted a lot of attention because of their flexible structure controllability, which can endow them with a variety of excellent properties. At present, benzoxazine resins have been widely used in electronic packaging materials, aerospace materials, high-end structural bonds and other fields as the matrix of composite materials or the main component of adhesives. [0003] In recent years, environmental problems have become more and more serious. With the rapid development of science and technology, people are paying more and more attention to the impact of the develo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G14/073C08G14/09C07D498/04
CPCC08G14/06C07D498/04
Inventor 张侃郝柏然杨蕊刘宇奇韩梦超
Owner JIANGSU UNIV
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