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Preparation method of high ceramization yield SiBNC precursor fiber

A precursor fiber and ceramization technology, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, single-component synthetic polymer rayon, etc., can solve the problems of high ceramization yield, low ceramization yield, unfavorable spinning, etc. problems, to achieve the effect of simple operation, easy access to raw materials, and simplified operation

Inactive Publication Date: 2017-06-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantages of this method are: the raw materials are easy to obtain, and the high temperature resistance is good; the disadvantages are: the multi-step method is cumbersome to operate and the ceramicization yield is low
The advantages of this method are: the precursor has a high degree of crosslinking, and the ceramic yield is high; the disadvantage is: the precursor product is insoluble in common organic solvents, the extraction and purification method is cumbersome to operate, and the product yield is low, which is not suitable for mass preparation of the precursor
The advantage of this method is: the reaction steps are simple; the disadvantage is: directly use NH 3 Provide nitrogen source, the degree of cross-linking is difficult to control, which is not conducive to spinning

Method used

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  • Preparation method of high ceramization yield SiBNC precursor fiber
  • Preparation method of high ceramization yield SiBNC precursor fiber
  • Preparation method of high ceramization yield SiBNC precursor fiber

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Replace the double-layer reactor with a stirring paddle with nitrogen with a purity of 99.99%, use n-hexane as a solvent, SiCl 4 、BCl 3 and CH 3 NH 2 as raw material (SiCl 4 、BCl 3 and CH 3 NH 2 The molar ratio of the SiBNC precursor is 1:2:20), co-condensation at -20°C for 6h to synthesize the n-hexane solution of the SiBNC precursor small molecule; place the solution in a reaction vessel with a stirring and distillation device, and heat it in an oil bath The n-hexane solvent was distilled off at 85°C; after the solvent was distilled off, NH was bubbled into the precursor small molecule for 4 hours under nitrogen protection at 90°C 3 , to obtain the SiBNC precursor polymer, the average molecular weight of the polymer is 1000; the SiBNC precursor polymer is placed in the melt spinning equipment under the condition of 120 ℃ for vacuum defoaming for 4h, in nitrogen atmosphere, the temperature is 90 ℃, the pressure is SiBNC precursor fibers with a diameter of 70 μm ...

Embodiment 2

[0033] Replace the double-layer reactor with a stirring paddle with nitrogen with a purity of 99.99%, use n-hexane as a solvent, SiCl 4 、BCl 3 and CH 3 NH 2 as raw material (SiCl 4 、BCl3 and CH 3 NH 2 The molar ratio of the SiBNC precursor is 1:1:14), co-condensation at -30°C for 9h to synthesize the n-hexane solution of the small molecule of the SiBNC precursor; place the solution in a reaction vessel with a stirring and distillation device, and heat it in an oil bath to The n-hexane solvent was distilled off at 95°C; after the solvent was distilled off, NH was bubbled into the precursor small molecules for 6h under the condition of 100°C under the protection of nitrogen. 3 , to obtain the SiBNC precursor polymer, the average molecular weight of the polymer is 2000; the SiBNC precursor polymer is placed in the melt spinning equipment under the condition of 140 ℃ for vacuum defoaming for 6h, in nitrogen atmosphere, the temperature is 100 ℃, the pressure is SiBNC precurso...

Embodiment 3

[0035] Replace the double-layer reactor with a stirring paddle with nitrogen with a purity of 99.99%, use n-hexane as a solvent, SiCl 4 、BCl 3 and CH 3 NH 2 as raw material (SiCl 4 、BCl 3 and CH 3 NH 2 The molar ratio of the SiBNC precursor is 2:1:22), co-polycondensation at -40°C for 12h to synthesize the n-hexane solution of the small molecule of the SiBNC precursor; place the solution in a reaction vessel with a stirring and distillation device, and heat it in an oil bath to The n-hexane solvent was distilled off at 105°C; after the solvent was distilled off, NH was bubbled into the precursor small molecule for 8 hours under nitrogen protection at 110°C 3 , to obtain the SiBNC precursor polymer, the average molecular weight of the polymer is 2500; the SiBNC precursor polymer is placed in the melt spinning equipment under the condition of 160 ℃ for vacuum defoaming for 8h, in nitrogen atmosphere, the temperature is 110 ℃, the pressure is SiBNC precursor fibers with a ...

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Abstract

The invention relates to a preparation method of a high ceramization yield SiBNC precursor fiber. The preparation method comprises the following steps: performing copolycondensation on SiCl4, BCl3 and CH3NH2 used as raw materials, and purifying to obtain SiBNC precursor small molecules; blowing NH3 into the SiBNC precursor small molecules in a nitrogen atmosphere at 90-110 DEG C for 4-8 hours to obtain a SiBNC precursor polymer; and performing vacuum defoamation on the SiBNC precursor polymer, and performing melt spinning to obtain the high ceramization yield SiBNC precursor fiber. The method provided by the invention is simple to operate, solves the problems of low ceramization yield, low strength and the like of the SiBNC precursor fiber in the prior art, and lays a foundation for continuous preparation of the high ceramization yield SiBNC precursor fiber.

Description

technical field [0001] The invention belongs to the field of preparation of ceramic fibers, in particular to a method for preparing SiBNC precursor fibers with high ceramicization yield. Background technique [0002] SiBNC ceramic fiber has excellent ablation resistance, high temperature oxidation resistance, high temperature creep resistance, high temperature strength and modulus retention, etc. It can be amorphized below 1700 ° C, and its oxidation resistance in air at 1700 ° C is far better than Better than SiC or Si 3 N 4 Ceramics have a very low weight loss rate at 2000°C and have very high structural stability. The preparation method of SiBNC ceramic fiber is mainly the precursor transformation method, but the ceramization yield of SiBNC precursor fiber reported in the literature is only between 40% and 70%, which also leads to the loss of the precursor fiber during the ceramization transformation process. Large and large voids lead to the problems of large defects ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/10D01F6/78
CPCD01F6/78D01F9/10
Inventor 余木火张晨宇刘勇韩克清常雪峰彭帅崔永杰
Owner DONGHUA UNIV