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Polybenzoxazine cross-linked hydrolysis-resistant polyborosiloxane and preparation method thereof

A technology of polybenzoxazine and polyborosiloxane, which is applied in the field of new polyborosiloxane and its preparation, can solve problems such as poor hydrolysis resistance, achieve excellent hydrolysis resistance, simple and easy synthetic route, The effect of high Tg

Active Publication Date: 2019-12-06
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Aiming at the deficiencies of the prior art, especially the defect of poor hydrolysis resistance of the existing polyborosiloxane, the present invention provides a polybenzoxazine-crosslinked hydrolysis-resistant polyborosiloxane and a preparation method thereof

Method used

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  • Polybenzoxazine cross-linked hydrolysis-resistant polyborosiloxane and preparation method thereof
  • Polybenzoxazine cross-linked hydrolysis-resistant polyborosiloxane and preparation method thereof
  • Polybenzoxazine cross-linked hydrolysis-resistant polyborosiloxane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Example 1. Synthesis of silicon-containing benzoxazine monomers based on phenol and γ-aminopropylmethyldimethoxysilane

[0070] Dissolve 0.25g of paraformaldehyde and 0.75g of γ-aminopropylmethyldimethoxysilane in 20mL of dioxane, stir the reaction at room temperature for 0.5h, add 0.44g of phenol, raise the temperature to 90°C, and react for 24h . Post-treatment: the solvent was removed by rotary evaporation, and the crude product was vacuum-dried at 60° C. to obtain a yellow liquid with a yield of 80%.

Embodiment 2

[0071] Example 2. Synthesis of silicon-containing benzoxazine monomers based on phenol and γ-aminopropylmethyldiethoxysilane

[0072] Dissolve 0.25g of paraformaldehyde and 0.51g of γ-aminopropylmethyldiethoxysilane in 20mL of dioxane, stir and mix at room temperature for 0.5h, add 0.44g of phenol, raise the temperature to 80°C, and react for 10h . Post-processing: the solvent was removed by rotary evaporation, and the crude product was vacuum-dried at 60° C. to obtain a yellow liquid with a yield of 62%.

Embodiment 3

[0073] Example 3, Synthesis of silicon-containing benzoxazine monomers based on bisphenol A and γ-aminopropylmethyldiethoxysilane

[0074] Dissolve 0.25g of paraformaldehyde and 0.51g of γ-aminopropylmethyldiethoxysilane in 20mL of dioxane, stir and mix at room temperature for 0.5h, add 0.64g of bisphenol A, and raise the temperature to 80°C. Reaction 10h. Post-processing: the solvent was removed by rotary evaporation, and the crude product was vacuum-dried at 60° C. to obtain a yellow liquid with a yield of 60%.

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Abstract

The invention relates to polybenzoxazine cross-linked hydrolysis-resistant polyborosiloxane and a preparation method thereof. The preparation method comprises: sequentially adding phenol, formaldehyde, amine and an organic solvent into a reaction bottle, heating and stirring for a certain time, cooling to a room temperature after the reaction is completed, and carrying out rotary evaporation to remove the organic solvent to obtain a silicon-containing benzoxazine monomer; carrying out a reaction on the obtained benzoxazine monomer and a boron-containing compound to obtain a borosiloxane prepolymer containing a benzoxazine side group; and carrying out thermocuring cross-linking on the obtained prepolymer to obtain the polybenzoxazine cross-linked hydrolysis-resistant polyborosiloxane. According to the present invention, the polybenzoxazine cross-linked hydrolysis-resistant polyborosiloxane hybrid material is prepared by linking the benzoxazine side group to the borosiloxane, such that the problem of easy hydrolysis of the common polyborosiloxane is successfully solved.

Description

technical field [0001] The invention relates to a polybenzoxazine cross-linked novel polyborosiloxane hybrid material, in particular to a hydrolysis-resistant novel polyborosiloxane and its preparation. Background technique [0002] Polyborosiloxane (referred to as PBS) refers to a polymer obtained by replacing some silicon atoms in the polysiloxane skeleton with boron atoms. Its molecular formula is as follows: [0003] [0004] Among them, R 1 , R 2 For alkyl, aryl, hydrogen, oxygen, etc., R 3 For oxygen, aryl, etc. [0005] In the PBS molecular chain, the bond energies of B-O and Si-O are as high as 537.6kJ / mol and 422.5kJ / mol respectively, and there are p-π and d-π conjugation effects. These factors make some varieties of PBS commonly used at temperatures It can reach 450°C, and the maximum operating temperature can reach 550°C, and its heat resistance is much higher than that of conventional polyimide (commonly used at 200°C, with a maximum of 250°C). The cerami...

Claims

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Application Information

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IPC IPC(8): C08G79/08C07F7/18
CPCC07F7/1892C08G79/08
Inventor 鲁在君高生孙露露
Owner SHANDONG UNIV
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