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A kind of preparation method of high temperature resistant phenolic resin with organic silicon resin as curing agent

A phenolic resin and organosilicon technology, applied in the field of high temperature resistant phenolic resin preparation, can solve the problems of no significant improvement in corrosion resistance, low peel strength, etc. strong effect

Active Publication Date: 2019-12-31
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the material peel strength is low and the corrosion resistance is not significantly improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Put the polysilazane resin precursor in a container, heat it to 120° C. in an oil bath under the protection of nitrogen, and stir for 6 hours to obtain a polysilazane resin prepolymer with a crosslinking degree of 10%;

[0023] (2) Mix the polysilazane resin prepolymer obtained in step (1) with the phenolic resin under nitrogen protection at a mass ratio of 1:10 at 80°C, and then inject the mixed solution into the mold cavity, And maintain a negative pressure of -0.06MPa at 60°C for 30min, then perform curing treatment, vacuumize at room temperature, raise the temperature to 100°C at a heating rate of 15°C / min, and keep it for 1.5h; then use a heating rate of 3°C / min , the temperature was raised to 130°C, the pressure was 0.3MPa, and the temperature was kept for 2 hours; then the pressure was increased to 0.6MPa; the temperature was raised to 180°C at a heating rate of 5°C / min, and the mold was released after holding for 2 hours to obtain a high temperature resistant...

Embodiment 2

[0026] (1) Put the polycarbosilane resin precursor in a container, heat it to 140° C. in an oil bath under the protection of nitrogen, and stir for 4 hours to obtain a polycarbosilane resin prepolymer with a crosslinking degree of 15%;

[0027] (2) Mix the polycarbosilane resin prepolymer obtained in step (1) with the phenolic resin under nitrogen protection at a mass ratio of 2:10 at 83°C, then inject the mixture into the mold cavity, and Maintain a negative pressure of -0.07MPa at 70°C for 25min, then perform curing treatment, vacuumize at room temperature, raise the temperature to 110°C at a heating rate of 17°C / min, and keep it for 1h; then heat up at a heating rate of 4°C / min To 140°C, the pressure is 0.3MPa, and keep warm for 1.5h; then increase the pressure to 0.5MPa; raise the temperature to 185°C at a heating rate of 7°C / min, keep warm for 1.5h, and release the mold to obtain a high temperature resistant phenolic resin.

[0028] Using the silicone resin prepared in th...

Embodiment 3

[0030] (1) Put the polysilaborazane resin precursor in a container, heat to 165° C. in an oil bath under the protection of nitrogen, and stir for 2 hours to obtain a polysilaborazane resin prepolymer with a crosslinking degree of 20%;

[0031] (2) Mix the polysilaborazane resin prepolymer obtained in step (1) with the phenolic resin under nitrogen protection at a mass ratio of 3:10 at 85°C, and then inject the mixture into the mold cavity , and maintain a negative pressure of -0.08MPa at 80°C for 20min, then perform curing treatment, vacuumize at room temperature, raise the temperature to 110°C at a heating rate of 20°C / min, and keep it for 1h; then use a heating rate of 5°C / min , the temperature was raised to 150°C, the pressure was 0.3MPa, and the temperature was kept for 1h; then the pressure was increased to 0.4MPa; the temperature was raised to 190°C at a heating rate of 10°C / min, and the high temperature resistant phenolic resin was obtained by demolding after holding for...

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Abstract

The invention relates to a method for preparing high-temperature resistant phenolic resin with organic silicon resin as a curing agent. The method comprises the following steps: heating an organic silicon resin precursor in an oil bath under nitrogen protection, and stirring to react to obtain organic silicon resin prepolymer having a crosslinking degree of 10-20 percent; heating and uniformly mixing with phenolic resin in a mass ratio of (0.1-0.3):1 in under nitrogen protection, injecting the mixed solution into a mold cavity, and reacting at negative pressure; and curing, and removing the mold to obtain the high-temperature resistant phenolic resin. The preparation method is simple in process and strong in operability, is free of overflow of small molecules in the curing process, and is applicable to industrial production. By adopting the method, organic silicon resin is selected as a curing agent, and the cured phenolic resin has strong instant heat resistance, and has relatively high mechanical performance retention rate and residual carbon rate at high temperature.

Description

technical field [0001] The invention belongs to the technical field of phenolic resin preparation, and in particular relates to a preparation method of a high-temperature-resistant phenolic resin using organic silicon resin as a curing agent. Background technique [0002] Phenolic resin is a kind of artificial synthetic resin made by condensation reaction of phenolic compound and aldehyde compound. Because of its good electrical insulation performance, mechanical performance, ablation resistance, corrosion resistance and high heat resistance and With good water resistance, it is widely used in electrical and electronic, automobile manufacturing and machinery industries. Due to the presence of easily oxidized phenolic hydroxyl groups and methylene groups on the structure of phenolic resin, its heat resistance and oxidation resistance are limited. The heat resistance of ordinary phenolic resin can no longer meet its use in aerospace and other fields. When the temperature exce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/28
CPCC08G8/28
Inventor 刘勇刘泽新刘涛纪宝明
Owner DONGHUA UNIV
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