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Submicron heterocyclic aramid fiber and preparation method thereof

A technology for spinning heterocyclic aramid fibers and heterocyclic aramid fibers, which is applied in the directions of fiber treatment, spinning solution preparation, fiber chemical characteristics, etc., can solve the problems of high hardness and large size of heterocyclic aramid fibers, and achieve excellent flexibility. performance, low equipment requirements, and the effect of reducing surface tension

Active Publication Date: 2022-07-01
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] This application provides a submicron heterocyclic aramid fiber and its preparation method, aiming to solve the problem of large size and high hardness of heterocyclic aramid fiber

Method used

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  • Submicron heterocyclic aramid fiber and preparation method thereof
  • Submicron heterocyclic aramid fiber and preparation method thereof
  • Submicron heterocyclic aramid fiber and preparation method thereof

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preparation example Construction

[0036] Preparation method of heterocyclic aramid fiber spinning solution

[0037] The embodiment of the first aspect of the present application provides a preparation method of a submicron heterocyclic aramid fiber, comprising:

[0038] S10. The step of preparing a polymer includes performing solution polymerization of a diamine monomer and a diacid chloride in a mixed solution of an organic solvent and an inorganic compound to obtain a polymer; wherein the diamine monomer includes a first diamine monomer and a second diamine monomer, the first diamine monomer is a heterocyclic diamine, the second diamine monomer is an aromatic ring diamine, and the molar concentration of the diamine monomer is 0.05-0.5 mol / L;

[0039] S20. The step of preparing a spinning solution for heterocyclic aramid fiber, comprising dissolving the polymer in a spinning solvent containing a viscosity modifier to obtain a spinning solution for heterocyclic aramid fiber, wherein the heterocyclic aramid f...

Embodiment 1

[0100] Under nitrogen protection, the dewatered N,N-dimethylacetamide was mixed with lithium chloride, stirred to dissolve the lithium chloride, and cooled to 10°C in a cold water bath to obtain a mixed solution, wherein N,N- The weight ratio of dimethylacetamide to lithium chloride was 50:1.75.

[0101] P-phenylenediamine and 2-(4-aminophenyl)-5-aminobenzimidazole are added to the mixed solution, and the molar concentration of the diamine monomer in the mixed solution is 0.15mol / L, wherein p-phenylenediamine and The molar ratio of 2-(4-aminophenyl)-5-aminobenzimidazole was 1:2. After the diamine monomer was dissolved, it was cooled to 0°C, and then terephthaloyl chloride was added. The molar ratio of the structural unit of the diacid chloride and the structural unit of the diamine was 1.01:1, and the polymerization reaction was carried out with high-speed stirring, and the stirring speed was 500rpm. , the reaction time was 45 min, and the polymer was obtained.

[0102] N,N-...

Embodiment 2

[0105] Under nitrogen protection, the dewatered N,N-dimethylformamide was mixed with calcium chloride, stirred to dissolve calcium chloride, and cooled to 10°C in a cold water bath to obtain a mixed solution, wherein N,N- The weight ratio of dimethylformamide to calcium chloride was 50:3.

[0106] 5-chloro-p-phenylenediamine and 2-(4-aminophenyl)-5-aminobenzimidazole are added to the mixed solution, and the molar concentration of the diamine monomer in the mixed solution is 0.3 mol / L, wherein 5 - The molar ratio of chloro-p-phenylenediamine and 2-(4-aminophenyl)-5-aminobenzimidazole is 1:2. After the diamine monomer is dissolved, it is cooled to 0 °C, and then terephthaloyl chloride is added. The molar ratio of the structural unit of diacid chloride and the structural unit of diamine is 1:1, and the polymerization reaction is carried out with high-speed stirring, and the stirring speed is 1000rpm. , the reaction time is 30min, and the polymer is obtained.

[0107] N,N-dimeth...

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Abstract

The invention discloses a submicron heterocyclic aramid fiber and a preparation method thereof. By regulating and controlling the raw material adding proportion, reaction parameters and the viscosity of the obtained polymer in the diamine monomer and diacyl chloride polymerization process, the surface tension of the heterocyclic aramid fiber spinning solution and the extrusion swelling effect during spinning are greatly reduced, and the stability and spinnability of the heterocyclic aramid fiber spinning solution are improved; spinning the heterocyclic aramid fiber spinning solution through an air flow spinning process to finally obtain the submicron fiber with the diameter of 100 nm to 1 mu m, and the fiber has excellent flexibility; and finally, the submicron heterocyclic aramid fiber can be prepared into different material forms through different collection modes, which is beneficial to widening the processing mode and application field of a later product. The preparation method of the submicron heterocyclic aramid fiber provided by the invention is simple in process, energy-saving, environment-friendly, efficient and low in equipment requirement, can be well compatible with the existing process, and has great large-scale application potential.

Description

technical field [0001] The application belongs to the technical field of preparation of heterocyclic aramid fibers, and in particular relates to a submicron heterocyclic aramid fiber and a preparation method thereof. Background technique [0002] Heterocyclic aramid fiber has the properties of light weight, high strength, high toughness, heat resistance, flame retardant and excellent wave-transmitting insulation, etc. It can be used as a multi-purpose composite material integrating bulletproof, stealth and other functions. It has important application value in the fields of aerospace, national defense and military industry. [0003] However, due to the influence of the viscosity, stability and spinning technology of the heterocyclic aramid spinning solution, the current heterocyclic aramid fibers mainly exist in the form of micron-sized fibers, and the hardness of the micron-sized heterocyclic aramid fiber fabrics is relatively high. high, and it is difficult to prepare sma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/90D01F1/02C08G69/32C08G69/28D01D1/02D01D1/10D01D5/14
CPCD01F6/905D01F1/02C08G69/32C08G69/28C08G69/265D01D1/02D01D1/106D01D1/103D01D5/14
Inventor 庹新林杨诗煊
Owner TSINGHUA UNIV
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