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Method for synthesizing novel spinnable polyborazane precursor in one pot

A technology of polyborazane and synthesis method, applied in textiles and papermaking, chemical characteristics of fibers, etc., can solve the problems of difficult spinning, low ceramic yield, high system viscosity, etc., and achieve excellent spinnability and low oxygen content. , the effect of simple preparation process

Active Publication Date: 2021-02-09
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a method for synthesizing a novel spinnable polyborazane precursor in one pot, which is used to overcome the disadvantages of the precursor synthesized in the prior art having a network structure, high viscosity of the system, difficult spinning, and low ceramic yield.

Method used

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  • Method for synthesizing novel spinnable polyborazane precursor in one pot
  • Method for synthesizing novel spinnable polyborazane precursor in one pot
  • Method for synthesizing novel spinnable polyborazane precursor in one pot

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Embodiment 1

[0048] This embodiment provides a method for one-pot synthesis of novel spinnable polyborazane precursors, including:

[0049] (1) prepare MAB monomer and RAB monomer;

[0050] S11: Determine the copolymerization ratio of MAB and RAB in the target product to 10:1;

[0051] S12: According to the copolymerization ratio of 10:1, set the molar ratio of TCB, n-propylamine and methylamine to 11:1:32;

[0052]S13: Dissolve TCB in toluene, add triethylamine and n-propylamine under the condition of <-10°C, stir for 1 hour, then feed methylamine gas, continue stirring for 8 hours under the condition of <-10°C, and then lower the temperature from < Warm up to room temperature at -10°C, stir for 8 hours, and vacuum filter to obtain a colorless mixed monomer liquid of MAB and RAB;

[0053] (2) Preparation of novel spinnable polyborazane (PRMAB) precursor;

[0054] The colorless mixed monomer liquid of MAB and RAB was heated up to 140°C, kept at 140°C for 2h, and cooled naturally to room...

Embodiment 2

[0057] This embodiment provides a method for one-pot synthesis of novel spinnable polyborazane precursors, including:

[0058] (1) prepare MAB monomer and RAB monomer;

[0059] S11: Determine the copolymerization ratio of MAB and RAB in the target product to 4:1;

[0060] S12: According to the copolymerization ratio of 4:1, set the molar ratio of TCB, n-propylamine and methylamine to 5:1:14;

[0061] S13: Dissolve TCB in a mixture of toluene and xylene, add triethylamine and n-propylamine at <-10°C, stir for 2 hours, then inject methylamine gas, and continue stirring for 6 hours at <-10°C , then raise the temperature from <-10°C to room temperature, stir for 6 hours, and vacuum filter to obtain a colorless mixed monomer liquid of MAB and RAB;

[0062] (2) Preparation of novel spinnable polyborazane (PRMAB) precursor;

[0063] The colorless mixed monomer liquid of MAB and RAB was heated up to 140°C, kept at 140°C for 4h, and cooled naturally to room temperature to obtain a n...

Embodiment 3

[0066] This embodiment provides a method for one-pot synthesis of novel spinnable polyborazane precursors, including:

[0067] (1) prepare MAB monomer and RAB monomer;

[0068] S11: Determine the copolymerization ratio of MAB and RAB in the target product to 1:4;

[0069] S12: According to the copolymerization ratio of 4:1, set the molar ratio of TCB, n-propylamine and methylamine to 5:4:11;

[0070] S13: Dissolve TCB in chlorobenzene, add triethylamine and n-propylamine under the condition of <-10°C, stir for 3 hours, then introduce methylamine gas, continue stirring for 4 hours under the condition of <-10°C, and then lower the temperature from <-10°C, warm up to room temperature, stir for 6 hours, and vacuum filter to obtain a colorless mixed monomer liquid of MAB and RAB;

[0071] (2) Preparation of novel spinnable polyborazane (PRMAB) precursor;

[0072] The colorless mixed monomer liquid of MAB and RAB was heated to 180°C, kept at 180°C for 6h, and cooled naturally to ...

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Abstract

The invention discloses a method for synthesizing a novel spinnable polyborazine precursor in one pot, which comprises the following steps: determining the copolymerization ratio x:y of MAB to RAB ina target product, setting the molar ratio of TCB to alkylamine to methylamine according to the copolymerization ratio x:y, and synthesizing MAB and RAB monomers in the ratio x:y by using trichloroborazine as a raw material, thereby obtaining the novel spinnable polyborazine precursor; finally, carrying out polymerization on the MAB monomer and the RAB monomer at the temperature of 140-220 DEG C toobtain the novel spinnable polyborazane precursor. According to the method, two monomers can be prepared in the same container, copolymerization can be achieved without transferring, the method has the advantages of being simple in preparation process and convenient to implement on a large scale, the prepared novel spinnable polyborazane precursor ceramic is high in yield and low in oxygen content, the precursor has excellent spinnability, and the spinning length can reach larger than 1000 m.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a method for synthesizing novel spinnable polyborazane precursors in one pot. Background technique [0002] Boron nitride fibers have excellent properties such as high temperature resistance and chemical corrosion resistance, as well as excellent dielectric properties, good electrical insulation, and good thermal conductivity. They have broad application prospects in cutting-edge technical fields such as aviation, aerospace, electric power, and electronics. Boron nitride fiber was first described by Economy et al. 2 o 3 Fiber in NH 3 B at the center during nitriding 2 o 3 Nitriding treatment synthesis is carried out in the atmosphere, but it is difficult to obtain homogeneous boron nitride fibers, resulting in poor fiber performance. The boron nitride fiber prepared by organic precursor conversion method has become the main method used in the research of boron nitr...

Claims

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Application Information

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IPC IPC(8): C08G79/08C04B35/58D01F9/10
CPCC08G79/08C04B35/583D01F9/10
Inventor 王兵王应德邵长伟王小宙苟燕子韩成龙鑫杜贻昂李威
Owner NAT UNIV OF DEFENSE TECH
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