Novel silicon-containing benzoxazine and preparation method thereof

A new type of benzoxazine technology, applied in the field of new benzoxazine monomers and their polymers, can solve the problems of insufficient flame retardancy and dielectric properties, poor mechanical properties, poor thermal stability, etc., and achieve excellent Effects of thermal stability and mechanical properties, good thermal stability, and excellent dielectric properties

Active Publication Date: 2018-01-26
SOUTHWEST PETROLEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Another purpose of the present invention is to solve the technical problems of existing silicon-containing benzoxazines such as poor mechanical properties, poor thermal stability, insufficient flame retardancy and dielectric properties, and to provide a kind of benzoxazine with good thermal stability and high residual Silicon-containing benzoxazine

Method used

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  • Novel silicon-containing benzoxazine and preparation method thereof
  • Novel silicon-containing benzoxazine and preparation method thereof
  • Novel silicon-containing benzoxazine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] At room temperature, add 2.44g of bis(hydroxyphenyl)dimethylsilicon, 1.86ml of aniline and 1.23g of paraformaldehyde into a round bottom flask containing 30ml of chloroform. The molar ratio of aniline and paraformaldehyde is 1:2:4.1, and the reaction is heated under reflux for 1 day. After the reaction is complete, the chloroform is evaporated to dryness with a rotary evaporator, and the silicon-containing benzoxazine monomer is obtained by column chromatography. The reaction principle is:

[0040]

[0041] Pour 2g of the above-prepared silicon-containing benzoxazine monomer into a circular aluminum mold, place it in an electric thermostatic drying oven, and solidify in stages at different temperatures to obtain ring-opening polymerized polybenzoxazine. The temperature rise curing process The steps are as follows: first heat up to 200°C for thermal curing for 3 hours, then heat up to 220°C for 3 hours, and finally heat to 240°C for thermal curing for 3 hours.

Embodiment 2

[0043] At room temperature, add 2.44g of bis(hydroxyphenyl)dimethylsilicon, 1.86ml of aniline and 1.26g of paraformaldehyde into a round bottom flask containing 30ml of toluene, bis(hydroxyphenyl)dimethylsilicon, The molar ratio of aniline and paraformaldehyde is 1:2:4.2, and the reaction is heated and refluxed for 1 day. After the reaction is completed, the toluene is evaporated to dryness with a rotary evaporator, and the silicon-containing benzoxazine monomer is obtained by column chromatography. The reaction principle is:

[0044]

[0045] Pour 2g of the above-prepared silicon-containing benzoxazine monomer into a circular aluminum mold, place it in an electric thermostatic drying oven, and solidify in stages at different temperatures to obtain ring-opening polymerized polybenzoxazine. The temperature rise curing process It is: first heat up to 200°C for thermal curing for 3 hours, then heat up to 220°C for thermal curing for 3 hours, and finally heat to 240°C for thermal cur...

Embodiment 3

[0047] At room temperature, add 2.44g of bis(hydroxyphenyl)dimethylsilicon, 1.86ml of aniline and 1.29g of paraformaldehyde into a round-bottomed flask containing 30ml of benzene, bis(hydroxyphenyl)dimethylsilicon, The molar ratio of aniline and paraformaldehyde is 1:2:4.3, and the reaction is heated and refluxed for 1 day. After the reaction is completed, the benzene is evaporated to dryness with a rotary evaporator, and the silicon-containing benzoxazine monomer is separated by column chromatography. The reaction principle is:

[0048]

[0049] Pour 2g of the above-prepared silicon-containing benzoxazine monomer into a circular aluminum mold, place it in an electric thermostatic drying oven, and solidify in stages at different temperatures to obtain ring-opening polymerized polybenzoxazine. The temperature rise curing process It is: first heat up to 200°C for thermal curing for 3 hours, then heat up to 220°C for thermal curing for 3 hours, and finally heat to 240°C for thermal ...

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Abstract

The invention discloses a novel silicon-containing benzoxazine monomer and a preparation method thereof. The silicon-containing benzoxazine monomer is synthesized through reaction of silicon-containing diphenol, an amine compound and paraformaldehyde under a solvent reflux condition; and silicon-containing diphenol is prepared through reaction of phenol halide and chlorosilane. The preparation method of the silicon-containing benzoxazine monomer comprises the steps of adding silicon-containing diphenol, the amine compound and paraformaldehyde into a round-bottom flask containing benzene, methylbenzene or chloroform, carrying out heating reflux, and after the reaction is complete, separating, so as to obtain the silicon-containing benzoxazine monomer. The silicon-containing benzoxazine monomer is put into a round aluminum mold, the round aluminum mold is put into an electric-heating constant-temperature drying tank and is cured at different temperatures in different stages in the electric-heating constant-temperature drying tank, and then ring-opening polymerized polybenzoxazine is obtained. The silicon-containing benzoxazine has high heat stability and carbon residue rate, excellent flame retardance, dielectric property and corrosion resistance and can be applied to the fields of ablation-resistant materials, flame-retardant materials, anti-corrosion materials, electronic packaging and the like.

Description

Technical field [0001] The invention relates to a new type of benzoxazine monomer and its polymer, in particular to a silicon-containing benzoxazine monomer, polybenzoxazine and a corresponding preparation method. Background technique [0002] Benzoxazine is a new type of resin developed on the basis of traditional phenolic resin. It is a six-membered heterocyclic compound obtained by Mannich condensation reaction of phenols, formaldehyde or paraformaldehyde, and primary amines. Compared with other thermosetting resins (such as epoxy resin, phenolic resin, bismaleimide resin, etc.), the benzoxazine resin produced by the high-temperature ring-opening polymerization of benzoxazine has traditional Phenolic resin has high temperature resistance, flame retardancy, good dielectric and mechanical properties, and also has high carbon residue rate, high glass transition temperature, good dimensional stability, does not require catalysts during curing, no small molecules are released, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08C08G73/06
Inventor 李辉李云涛曾凯徐计雷李高旭
Owner SOUTHWEST PETROLEUM UNIV
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