Full-bio-based benzoxazine resin and preparation method thereof

A technology of benzoxazine and oxazine resin, applied in the field of materials, can solve the problems of non-environmental protection and sustainable development, achieve glass transition temperature and thermal stability improvement, natural and easy-to-obtain raw materials, and flame retardant The effect of performance improvement

Pending Publication Date: 2020-05-29
淮北绿洲新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lin uses aniline from petroleum resources as an amine source, which is not environmentally friendly and sustainable for development
Moreover, for the p

Method used

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  • Full-bio-based benzoxazine resin and preparation method thereof
  • Full-bio-based benzoxazine resin and preparation method thereof
  • Full-bio-based benzoxazine resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Preparation of bisphenols with vanillin / p-hydroxyacetophenone type chalcone structure:

[0045]Add 13.6g of vanillin (0.1mol) and 15.3g of p-hydroxyacetophenone (0.1mol) into the reaction vessel, add 50mL of toluene to dissolve, 2mL of boron trifluoride ether as catalyst, react at 55°C for 4h, and put The reaction solution was poured into methanol / water=1:1 (v / v) mixed solution for recrystallization to obtain golden yellow crystals, which were dried to obtain bisphenol powder with chalcone structure.

[0046] Such as figure 1 Shown is the infrared spectrogram of the vanillin / p-hydroxyacetophenone type chalcone structure bisphenol prepared in this embodiment, 3410cm -1 Represents the characteristic absorption peak of phenol-OH, 1640cm -1 Represents the characteristic absorption peak of C=O, 1593cm -1 Represents C=C, 1234cm -1 Representative-OCH 3 In summary, it shows that the synthetic product of this example is vanillin / p-hydroxyacetophenone bisphenol with chalcone...

Embodiment 2

[0048] Preparation of bisphenols with vanillin / p-hydroxyacetophenone type chalcone structure:

[0049] Add 13.6g vanillin (0.1mol) and 15.3g p-hydroxyacetophenone (0.1mol) to the reaction vessel, add 50mL toluene / ethanol (2:1v / v) mixed solution to dissolve, 2mL boron trifluoride ether as catalyst , reacted at 55°C for 4h, after the reaction was completed, the reaction solution was poured into methanol / water=1:1 (v / v) mixed solution for recrystallization to obtain golden yellow crystals, and chalcone structure bisphenol powder was obtained after drying.

Embodiment 3

[0051] Preparation of all biobased benzoxazine monomers:

[0052] Add 8.10g (0.03mol) of bisphenols with chalcone structure prepared in Example 1, 3.88g (0.04mol) of furfurylamine, and 3.60g (0.12mol) of paraformaldehyde into a mixture equipped with a condenser, a magnetic stirrer, and a thermometer. In a 250mL three-necked flask, the molar ratio of phenolic hydroxyl group, amino group and aldehyde group functional group is 6:4:12, then add 75mL of toluene solvent, mix well and heat to 115°C for 8 hours, after the reaction, pour the reaction solution into 100mL Precipitate in methanol solution to obtain a brown-yellow suspension, let it stand for 12 hours, remove the supernatant to obtain a brown-yellow precipitate, vacuum-dry the brown-yellow precipitate at 60°C for 8 hours, and finally grind the dried product to obtain a brown-yellow powder. It is a fully bio-based benzoxazine monomer.

[0053] Such as figure 2 Shown is the infrared spectrogram of the whole bio-based benz...

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Abstract

The invention discloses a full-bio-based benzoxazine resin and a preparation method thereof. The preparation method comprises the following steps: mixing bisphenol with a chalcone structure, furfurylamine and an aldehyde compound in an organic solvent, reacting for 8-48 hours at a temperature of 75-115 DEG C, purifying the reaction product to obtain a full-bio-based benzoxazine monomer; and curing the benzoxazine monomer at a temperature of 80-260 DEG C for 1-24 hours to obtain the full-bio-based benzoxazine resin; or irradiating the benzoxazine monomer by ultraviolet light for 0.5-4 hours, and curing the benzoxazine monomer for 4-24 hours at a temperature of 80-140 DEG C to obtain the full-bio-based benzoxazine resin. The curing temperature of the benzoxazine monomer containing a chalcone structure is further reduced; the thermal performance and crosslinking degree of the obtained benzoxazine resin are improved, and the obtained resin has a high glass transition temperature (204-376DEG C), a high carbon residue rate (50-70%), a high limit oxygen index (30.3-42.2) and a low dielectric constant (2.0-2.9).

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to an all-bio-based benzoxazine monomer, a resin and a preparation method thereof. Background technique [0002] Benzoxazine resin is a new type of phenolic resin, which is a six-membered heterocyclic compound synthesized from phenolic compounds, amine compounds and aldehyde compounds through Mannich reaction and cured at high temperature. While maintaining the excellent thermal properties, flame retardancy and electrical insulation of traditional phenolic resins, it also has many advantages that traditional phenolic resins do not have, such as no release of small molecules during processing and curing, and the product has low porosity. , The volume is close to zero shrinkage, and it has better high temperature thermal stability, flame retardancy, mechanical properties, chemical stability and low water absorption. In addition, there is no need for strong acid or stron...

Claims

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Application Information

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IPC IPC(8): C08G14/06
CPCC08G14/06
Inventor 曾鸣冯子健
Owner 淮北绿洲新材料有限责任公司
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