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Preparation method of liquid polyborosilazane

A technology of polyborosilazane and hexamethyldisilazane, which is applied in the field of preparation of liquid polyborosilazane, can solve the problems of complex process, high cost, and long synthesis steps of polymer route

Pending Publication Date: 2022-08-02
福建立亚化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polymer route has long synthesis steps, complicated process and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) The reaction kettle was heated to 100°C, vacuumed to -0.095MPa, and then kept for 3 hours. The reaction kettle was dried to remove moisture, and then nitrogen was introduced. Then, the reaction kettle was evacuated to <-0.09MPa, and the operation was repeated three times. Then, nitrogen was introduced and the temperature was lowered to keep the reaction kettle in a slightly positive pressure state.

[0026] (2) adding n-hexane to the reactor, cooling the reactor to -20°C, slowly feeding the boron chloride gas into the n-hexane, opening the stirring device of the reactor after adding, fully stirring to make the boron chloride dissolved in n-hexane. Then continue to add methyl hydrogen dichlorosilane and methyl vinyl dichlorosilane to the reactor, and fully stir and mix;

[0027] The molar mass ratio of n-hexane and boron chloride is 5:1. The molar mass ratio of methylhydrogendichlorosilane+methylvinyldichlorosilane to boron trichloride is 1:1.

[0028] (3) Control...

Embodiment 2

[0032] (1) The reaction kettle was heated to 125°C, vacuumed to -0.09MPa, and then closed for 2 hours, and the reaction kettle was dried to remove moisture. Then blow in nitrogen, then evacuate the reaction kettle to <-0.09MPa, and after repeated operations three times, introduce nitrogen and lower the temperature to keep the reaction kettle in a slightly positive pressure state.

[0033] (2) add toluene in the reaction kettle, cool the reaction kettle to -10 ℃, slowly pass the boron chloride gas into the toluene, open the stirring device of the reaction kettle after adding, fully stir to make the boron chloride dissolve in the toluene , then continue to add methylphenyldichlorosilane and methylpropargyldichlorosilane to the reactor, and fully stir and mix;

[0034] The molar mass ratio of toluene and boron chloride is 10:1. The molar mass ratio of methylphenyldichlorosilane+methylpropargyldichlorosilane to boron trichloride is 5:1.

[0035] (3) Controlling a certain flow ra...

Embodiment 3

[0040] (1) The reaction kettle was heated to 150°C, vacuumed to -0.08MPa, and then kept for 1 h, and the reaction kettle was dried to remove moisture. Then blow in nitrogen, then evacuate the reaction kettle to <-0.09MPa, and after repeated operations three times, introduce nitrogen and lower the temperature to keep the reaction kettle in a slightly positive pressure state.

[0041] (2) adding petroleum ether to the reaction kettle, cooling the reaction kettle to 0°C, slowly feeding boron chloride gas into the petroleum ether, opening the stirring device of the reaction kettle after adding, and stirring fully to dissolve the boron chloride in the petroleum ether In petroleum ether, then continue to add phenyl hydrogen dichlorosilane and methallyl dichlorosilane to the reactor, and fully stir and mix;

[0042] The molar mass ratio of petroleum ether to boron chloride is 1:1. The molar mass ratio of phenylhydrogendichlorosilane+methallyldichlorosilane to boron trichloride is 10...

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Abstract

The invention discloses a preparation method of liquid polyborosilazane, which comprises the following steps: heating a reaction kettle, replacing gas in the reaction kettle with nitrogen, and keeping the reaction kettle in a micro-positive pressure state; under the condition, sequentially adding a solvent, boron chloride gas, chlorosilane and unsaturated chlorosilane, and stirring to react; the invention discloses a preparation method of liquid polyborosilazane, which comprises the following steps of: adding a solvent into a mixed solution, dropwise adding hexamethyldisilazane into the mixed solution for reaction, distilling to remove the solvent, heating and distilling until no liquid flows out, and cooling a final product to obtain the liquid polyborosilazane, and adopts a one-step co-condensation method, so that the synthesis process of a precursor is greatly simplified, the synthesis process is simple, the synthesis yield is high, byproducts are easy to remove, and the preparation method is suitable for industrial production. The liquid polyborosilazane prepared by the method is adjustable in viscosity, and has the advantages of good wettability to fibers, high ceramic yield and the like.

Description

technical field [0001] The invention relates to the technical field of ceramic precursors, in particular to a preparation method of liquid polyborosilazane. Background technique [0002] Polyborosilazane (PBSZ) is the main polymer precursor for the preparation of high-performance silicon borocarbonitride (SiBCN) composite ceramics. SiBCN composite ceramics can be obtained by pyrolysis of PBSZ precursors. Due to the introduction of B, BN / B is formed during the ceramic transformation process. 4 C phase, therefore, SiBCN ceramic material has excellent high temperature thermal stability, oxidation resistance and creep resistance, and maintains amorphous form below 1700 ° C. It is one of the new generation of high-performance ceramic materials. It is used in aerospace and other high-tech The field has very broad application prospects. [0003] The preparation of ceramic matrix composites by the polymer precursor conversion method has a series of unique advantages: through the d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/62
CPCC08G77/62Y02E60/10
Inventor 郑桦贺卫东陈丽滨
Owner 福建立亚化学有限公司
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