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One-pot synthesis of novel spinnable polyborazane precursors

A technology of polyborazane and synthesis method, which is applied in the direction of textiles, papermaking, fiber chemical characteristics, etc., can solve the problems of high viscosity of the system, low ceramic yield, spinning difficulties, etc., and achieve low oxygen content, high yield, The effect of excellent spinnability

Active Publication Date: 2022-04-19
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • One-pot synthesis of novel spinnable polyborazane precursors
  • One-pot synthesis of novel spinnable polyborazane precursors
  • One-pot synthesis of novel spinnable polyborazane precursors

Examples

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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 polyborazane precursor in one pot. Firstly, the copolymerization ratio x:y of MAB and RAB in the target product is determined, and then TCB, alkylamine and formazan are set according to the copolymerization ratio x:y. According to the molar ratio of amines, trichloroborazine is used as raw material to synthesize MAB and RAB monomers with a ratio of x:y, and finally the MAB and RAB monomers are polymerized at 140-220°C to obtain a new type of spinnable polyboron nitrogen alkanes precursors. The method of the present invention can prepare two kinds of monomers in the same container and can realize copolymerization without transfer, and has the advantages of simple preparation process and convenient scale-up, and the prepared novel spinnable polyborazane precursor ceramic has high yield, The oxygen content is low, and the precursor has excellent spinnability, and the spinning length is >1000m.

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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Patent Type & Authority Patents(China)
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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