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Method for preparation of SiBN(C) ceramic fiber precursor by one-pot technique

A ceramic fiber and precursor technology, which is applied in the field of preparation of silicon boron nitrogen ceramic precursors, can solve the problems of high brittleness and low strength of ceramic fiber precursors, and achieve the effects of easy operation, brittleness and simple process

Active Publication Date: 2014-07-23
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the SiBN (C) ceramic fiber precursor has the disadvantages of high brittleness and low strength. The present invention aims at these deficiencies, and can prepare a SiBN (C) ceramic fiber precursor with good flexibility and high strength by adding comonomers for copolymerization. Laid the foundation for continuous spinning and pyrolysis of SiBN(C) ceramic fiber precursor

Method used

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  • Method for preparation of SiBN(C) ceramic fiber precursor by one-pot technique
  • Method for preparation of SiBN(C) ceramic fiber precursor by one-pot technique
  • Method for preparation of SiBN(C) ceramic fiber precursor by one-pot technique

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Embodiment 1

[0027] (1) Put 2L of anhydrous n-hexane into the reactor, and distill and clean the reactor at 85°C; (2) At -13°C, put 10L of anhydrous n-hexane into the reactor, and then pass into the liquid Methylamine 1.8L, then take MeHSiCl 2 3.75mol and 1mol / L BCl 3 Mix 2.5L of n-hexane solution evenly, and mix the mixed methyldichlorosilane and BCl 3 The solution is added into the anhydrous n-hexane solution of methylamine through an electromagnetic pump, and an exothermic reaction occurs in the container. The temperature in the reactor is controlled at -15 to -10°C by a circulating cooling pump. After the addition is completed, the reaction is carried out at room temperature for 24 hours. The obtained upper liquid is an anhydrous n-hexane solution of SiBN (C) ceramic fiber precursor molecules; (3) Take the n-hexane solution of SiBN (C) ceramic fiber precursor molecules obtained after the reaction in a three-necked flask, at Under the conditions, the n-hexane in the precursor molecule...

Embodiment 2

[0029] (1) Introduce 2L of anhydrous n-hexane into the reactor at a temperature of 85°C, and distill and clean the reactor; (2) Introduce 9L of anhydrous n-hexane into the reactor at -17°C, and then in liquid state Methylamine 1.5L, then take MeHSiCl 2 2.5mol and 1mol / L BCl 3 Mix 2.5L of n-hexane solution evenly, and mix the mixed methyldichlorosilane and BCl 3 The solution is added into the anhydrous n-hexane solution of methylamine through an electromagnetic pump, and an exothermic reaction occurs in the container. The temperature in the reactor is controlled at -20 to -15°C by a circulating cooling pump. After the addition is completed, the reaction is carried out at room temperature for 24 hours. The obtained upper liquid is an anhydrous n-hexane solution of SiBN (C) ceramic fiber precursor molecules; (3) Take the n-hexane solution of SiBN (C) ceramic fiber precursor molecules obtained after the reaction in a three-necked flask, at Under the conditions, the n-hexane in t...

Embodiment 3

[0031] (1) Introduce 2L of anhydrous n-hexane into the reactor at a temperature of 85°C, and distill and clean the reactor; (2) Introduce 9L of anhydrous n-hexane into the reactor at -17°C, and then in liquid state Methylamine 1.5L, then take MeHSiCl 2 2.5mol and 1mol / L BCl 3 Mix 2.5L of n-hexane solution evenly, and mix the mixed methyldichlorosilane and BCl 3The solution is added into the anhydrous n-hexane solution of methylamine through an electromagnetic pump, and an exothermic reaction occurs in the container. The temperature in the reactor is controlled at -20 to -15°C by a circulating cooling pump. After the addition is completed, the reaction is carried out at room temperature for 24 hours. The obtained upper liquid is an anhydrous n-hexane solution of SiBN (C) ceramic fiber precursor molecules; (3) Take the n-hexane solution of SiBN (C) ceramic fiber precursor molecules obtained after the reaction in a three-necked flask, at Under the conditions, the n-hexane in th...

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Abstract

The invention relates to a method for preparation of an SiBN(C) ceramic fiber precursor by a one-pot technique. The method includes: at a temperature ranging from -30DEG C to -10DEG C, synthesizing an anhydrous n-hexane solution of an SiBN(C) ceramic fiber precursor molecule from dichloromethylsilane, boron trichloride, methylamine and a solvent anhydrous n-hexane; under 70-120DEG C, removing n-hexane from the precursor molecule solution, then adding active group terminated polydimethyl siloxane, raising the temperature to 140-300DEG C, conducting heat preservation for 5-150h to obtain an SiBN ceramic fiber precursor polymer, and carrying out defoaming and melt spinning, thus obtaining the SiBN(C) ceramic fiber precursor. Compared with the existing synthesis methods, the method has the advantages of simple process and convenient operation, and preparation of the precursor can be completed by one-step reaction. The method provided by the invention can effectively solve the brittleness problem of the SiBN(C) ceramic fiber precursor, thus laying the foundation for continuous preparation and cracking of the SiBN(C) ceramic fiber precursor.

Description

technical field [0001] The invention belongs to the field of preparation of silicon boron nitrogen ceramic precursors, in particular to a method for preparing SiBN (C) ceramic fiber precursors in one pot. Background technique [0002] SiBN(C) ceramic fiber has both Si 3 N 4 The advantages of fiber and BN fiber can make up for the shortcomings of these two fibers at the same time, that is, it has high strength, high modulus, high temperature oxidation resistance, low dielectric constant, and excellent high temperature stability. It is a new type of ceramic material. It has become a new research hotspot in the field of ceramic materials in recent years, and has broad application prospects in national defense, aerospace, energy and other fields. [0003] Due to the extremely low diffusion coefficients of Si, B, etc. in nitrides and carbides, it is difficult to prepare SiBN(C) system ceramics by traditional powder sintering methods, and the precursor conversion method is an ef...

Claims

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Application Information

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IPC IPC(8): D01F8/16D01D5/08C08G77/60
Inventor 余木火王会峰牟世伟韩克清唐彬彬胡建建柯盛包邱显星贾军耿冉刘新东陈磊庄恒飞
Owner DONGHUA UNIV
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