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Preparation method for boron nitride ceramics fibre precursor

A technology of ceramic fibers and precursors, applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of unfavorable spinning process and high viscosity, and achieve the effects of good wave permeability, easy separation and good spinnability

Inactive Publication Date: 2009-02-18
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Over the past 10 years, foreign scholars have explored various ways to prepare BN precursors. In 1994, B.Bonnetot. reported a new process for preparing BN fibers using boron trichloride and methylamine to synthesize precursors, but the pioneer of this synthesis The body is a network structure with high viscosity, which is not conducive to the later spinning process

Method used

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  • Preparation method for boron nitride ceramics fibre precursor
  • Preparation method for boron nitride ceramics fibre precursor
  • Preparation method for boron nitride ceramics fibre precursor

Examples

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Comparison scheme
Effect test

Embodiment 1

[0027] A kind of preparation method of boron nitride ceramic fiber precursor, concrete steps are:

[0028] The first step: the anhydrous toluene solution of 40wt% cyclic trichloroborazane (36.3g) is cooled to -80°C with the PSL-1800 type magnetic stirring cryogenic tank, and 40wt% methylamine is added dropwise under magnetic stirring conditions. In anhydrous toluene solution, white flocculent methyl ammonium chloride precipitates immediately. After the dropwise addition, the temperature is raised to -40°C, reacted for 1 hour, then warmed up to room temperature, reacted for 10 hours, filtered to remove the precipitate, and used Rinse the precipitate with water toluene once, combine the filtrates, and heat up to 60°C under a vacuum of 3 mmHg to remove part of the toluene, wherein the weight ratio of methylamine to cyclic trichloroborazane is 3:10;

[0029] The second step: use PSL-1800 type magnetic stirring low temperature tank and tetrafluoroethylene tube to condense boron tri...

Embodiment 2

[0033] A kind of preparation method of boron nitride ceramic fiber precursor, concrete steps are:

[0034]The first step: the anhydrous toluene solution of 45wt% cyclic trichloroborazane (36.3g) is cooled to-70 ℃ with refrigeration equipment, and the anhydrous toluene solution of 45wt% methylamine is added dropwise under magnetic stirring conditions, immediately There is a white flocculent precipitate of methyl ammonium chloride. After the dropwise addition, the temperature is raised to 0°C, reacted for 10 hours, then warmed up to room temperature, reacted for 20 hours, filtered to remove the precipitate, and washed with anhydrous toluene for 8 times. Combine the filtrates, heat up to 30°C under a vacuum of 5 mmHg to remove part of the toluene, wherein the weight ratio of methylamine to cyclic trichloroborazane is 2:5;

[0035] The second step: use refrigeration equipment and tetrafluoroethylene tubes to condense boron trichloride into anhydrous toluene solution of 45wt% methy...

Embodiment 3

[0039] A kind of preparation method of boron nitride ceramic fiber precursor, concrete steps are:

[0040] The first step is to synthesize small molecule monomer 1 according to the following method: the anhydrous toluene solution of 43wt% cyclic trichloroborazane (36.3g) is cooled to -75°C with refrigeration equipment, and 43wt % methylamine in anhydrous toluene solution, white flocculent methyl ammonium chloride precipitates immediately, after the dropwise addition, heat up to -20°C, react for 5 hours, then warm up to room temperature, react for 15 hours, filter to remove Precipitate, and wash the precipitate with anhydrous toluene 4 times, combine the filtrate, and heat up to 40 ° C under a vacuum of 4 mm Hg to remove part of the toluene, wherein the weight ratio of methylamine to cyclic trichloroborazane is 7:20 . like figure 1 Shown is the infrared spectrum of the small molecule monomer 1 obtained in the first step; figure 2 It is the NMR boron spectrum of the small mo...

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Abstract

The invention relates to a method for preparing boron nitride ceramic fiber precursor polymer, the method comprises the following steps: the anhydrous toluene solution of cyclic trichloroboron azane is cooled to 80 DEG C below zero-70 DEG C below zero, anhydrous toluene solution of methylamine is dripped, and the reaction endures 1-10 hours under -40 DEG C below zero -0 DEG C, and then endures 10-20 hours under room temperature, and is subsequently filtered; the boron trichloride is condensed in anhydrous toluene solution of methylamine (40 DEG C below zero - 80 DEG C below zero), stirred for reaction for 1-10hr, and then stirred for 5-20hr under room temperature, and then filtered; the filtrates are combined, stirred for 2-4hr under 10 DEG C below zero -0 DEG C, stirred for 5-10hr under room temperature, and then filtered; the filtrates react for 10-60min under 50-100 DEG C, the toluene is evaporated out under 100-120 DEG C, and then react for 5-20hr under 160-170 DEG C. The precursor polymer synthesized by the method has a proper linear shape and a mesh structure, and has sound spinnability and wave-penetrating performance.

Description

technical field [0001] The invention relates to a preparation method of a boron nitride ceramic fiber precursor, belonging to the technical field of polymer materials. Background technique [0002] With the rapid development of modern high technology, especially the aerospace industry, the research and development of high-performance fibers, especially high-performance inorganic ceramic fibers, has become one of the focuses of material science research in the world today. Compared with some inorganic fibers, boron nitride fiber has high temperature and high strength, oxidation resistance, chemical corrosion resistance, low density, processability, self-lubricating, non-wetting with various metals, high dielectric properties, and good thermal conductivity And excellent characteristics such as excellent wave-transmitting performance. Its anti-oxidation temperature is higher than that of carbon fiber and boron fiber. It remains stable above 2500°C under inert conditions, and ...

Claims

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Application Information

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IPC IPC(8): C08G79/08D01F9/10
Inventor 余木火曹义苗韩克清李书同赵曦
Owner DONGHUA UNIV
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