Method for preparing ceramic fiber precursor

A ceramic fiber and precursor technology, applied in the field of polymer material preparation, can solve problems such as unfavorable spinning process and high viscosity

Inactive Publication Date: 2008-05-21
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Over the past ten years, foreign scholars have explored various ways to prepare BN precursors. B.Bonnetot. reported in Met.Chem.1994, 17, 583-593 that BN fibers were prepared by using boron trichloride and methylamine to synthesize precursors. A new process, but the precursor synthesized by this method has a network structure and high viscosity, which is not conducive to the later spinning process

Method used

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  • Method for preparing ceramic fiber precursor
  • Method for preparing ceramic fiber precursor
  • Method for preparing ceramic fiber precursor

Examples

Experimental program
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Effect test

Embodiment 1

[0025] (1) Preparation of small molecular monomers: Take 26.5ml (0.2mol) of a triethylamine solution (volume ratio 1:1) with a concentration of 7.55mol / l dimethylamine in a 250ml single-necked flask, and move the flask to PSL -1800 type magnetic stirring cryogenic tank, temperature -80°C, replace the air in the flask with nitrogen; condense 23.4g (0.2mol) of boron trichloride from the steel cylinder into the reaction vessel through the tetrafluoroethylene tube; after condensation, With magnetic stirring, react for 5 hours; rise to room temperature and stir for 1 hour to produce a yellow precipitate; filter under nitrogen protection, wash the precipitate several times with 50ml of anhydrous toluene, combine the washings and filtrate; transfer the filtrate and washings to a 250ml dry In the single-necked flask, still placed in a low-temperature tank at a temperature of -80°C, transfer 80ml of anhydrous toluene solution of methylamine (volume ratio: 1:1) into a 250ml constant pres...

Embodiment 2

[0029] (1) Preparation of small molecular monomers: take 30ml (0.15mol) of triethylamine solution with a concentration of 5mol / l diethylamine in a 250ml single-necked flask, and move the flask to a PSL-1800 type magnetic stirring low-temperature tank. -80°C, replace the air in the flask with argon; condense 17.55g (0.15mol) of boron trichloride from the steel cylinder into the reaction vessel through a tetrafluoroethylene tube; after condensation, with magnetic stirring, react for 10h; then Rise to room temperature and stir for 4 hours, producing a yellow precipitate; filter under argon protection, wash the precipitate several times with 50ml of n-hexane, combine the washings and filtrate; transfer the filtrate and washings to a 250ml dry single-necked flask, and keep at temperature In a low-temperature tank at -80°C, transfer 80ml of methylamine n-hexane solution (volume ratio: 1:1) into a 250ml constant pressure funnel, slowly add it dropwise into the flask, and stir it magne...

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Abstract

The invention relates to a preparation method of a ceramic fibre precursor. The steps comprises that (1) the preparation of a small molecular monomer: under the oxygen-free dry atmosphere under subzero 80 DEG C to 0 DEG C, the mol ratio of boron trichloride and aliphatic secondary amine is 1 to 0.2 to 1 to 1 to 5, the boron trichloride is slowly condensed into aliphatic secondary amine triethylamine solution to react for 1 to 20 hours under magnetic force mixing and then reacts for 1 to 20 hours under the room temperature to produce yellow sedimentation for filtering; then the mol ratio of anhydrous toluene solution and aliphatic primary amine is 1 to 1 to 5 to 1, the anhydrous toluene solution is added into the filtrate by dropping to react for 1 to 20 hours under subzero 80 DEG C to 0 DEG C along with magnetic force mixing and then reacts for 5 to 30 hours under the room temperature to produce the yellow sedimentation again for filtering and reduced pressure distillation;(2) the preparation of a BN precursor: the light yellow liquid is treated for multiple-stage linear heating under magnetic force mixing, the heating speed is 0.5 to 20 DEG C per minute, the liquid is heated till 150 DEG C to 180 DEG C for 15 to 25 hours and then cooled to obtain the yellow solid precursor. The technology of the method is simple, and the continuous industrialized production can be easily realized.

Description

technical field [0001] The invention belongs to the field of polymer material preparation, and in particular relates to a preparation method of a ceramic fiber precursor. Background technique [0002] 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. BN fiber has a variety of excellent properties, and has good composite compatibility with resins, metals, and ceramics. Boron nitride (BN) has many unique properties. It has a wide range of anti-electromagnetic radiation, low density, high temperature oxidation resistance, high heat of vaporization and excellent lubricating properties. Compared with graphite, BN has a small thermal expansion coefficient. And it can make oxide ceramics have good chemical inertness, which can be used as an ideal interface material, while BN fiber is expected to have high Young's modulus and high strength at t...

Claims

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Application Information

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IPC IPC(8): C04B35/622C04B35/583
Inventor 余木火谢伟炜韩克清李书同毕红艳曹建赵曦曹义苗
Owner DONGHUA UNIV
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