Preparation method for high-modulus para-aramid fiber

A para-aramid fiber and high modulus technology, which is applied in fiber treatment, fiber chemical characteristics, wet spinning, etc., can solve the problems of long drying time, more fluff, and low modulus, so as to reduce energy consumption, Improved fiber performance and high degree of continuity

Pending Publication Date: 2020-08-07
宁夏泰和芳纶纤维有限责任公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a preparation method of high-modulus para-aramid fiber. The present invention adopts low-temperature polycondensation, dry spray wet spinning, multi-stage drying technology, and optimizes equipment transformation, which can solve the problems of PPTA degradation, low modulus, and dryness. Problems such as long time and excessive wool can make high-modulus para-aramid fiber efficient, stable, and high-quality continuous production

Method used

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  • Preparation method for high-modulus para-aramid fiber
  • Preparation method for high-modulus para-aramid fiber

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Embodiment 1

[0020] A kind of preparation method of high modulus para-aramid fiber of the present invention: (1) preparation of polymer: under nitrogen protection, PPD is dissolved in NMP / CaCl 2 Stir and mix evenly in the solvent, use a condensing agent to control the temperature in the jacket of the reaction kettle at -5°C, add TPC twice, the molar ratio of TPC to PPD is 1.001:1, add 30% TPC for 8 seconds for the first time , then lower the temperature to -5~0°C, add 70% TPC for the second time to react for 30 minutes, transfer the reaction mixture to a neutralization tank and add 8% NaOH solution to neutralize it, and then use deionized Water graded washing 10 times, steam drying at 120°C to obtain PPTA with a water content of less than 100ppm and an intrinsic viscosity of 7.5-8.5dL / g;

[0021] (2) Preparation of spinning stock solution: at a temperature of 80-100°C, multi-stage jacket temperature control, under nitrogen sealing, mix and stir PPTA with an intrinsic viscosity of 7.5-8.5dL...

Embodiment 2

[0025] A kind of preparation method of high modulus para-aramid fiber of the present invention: (1) preparation of polymer: under nitrogen protection, PPD is dissolved in NMP / CaCl 2 Stir and mix evenly in the solvent, use a condensing agent to control the temperature in the jacket of the reaction kettle at -3°C, add TPC twice, the molar ratio of TPC to PPD is 1.001:1, add 40% TPC for 10 seconds for the first time , then lower the temperature to -5~0°C, add 60% TPC for the second time to react for 30 minutes, transfer the reaction mixture to a neutralization tank and add a 10% NaOH solution to neutralize it, and then use a deionized Water graded washing 10 times, steam drying at 130°C to obtain PPTA with a water content of less than 90ppm and an intrinsic viscosity of 7.5-8.5dL / g;

[0026] (2) Preparation of spinning stock solution: at a temperature of 80-100°C, multi-stage jacket temperature control, under nitrogen sealing, mix and stir PPTA with an intrinsic viscosity of 7.5-...

Embodiment 3

[0030] A kind of preparation method of high modulus para-aramid fiber of the present invention: (1) preparation of polymer: under nitrogen protection, PPD is dissolved in NMP / CaCl 2 Stir and mix evenly in the solvent, use a condensing agent to control the temperature in the jacket of the reaction kettle at -2°C, add TPC twice, the molar ratio of TPC to PPD is 1.002:1, add 45% TPC for 12 seconds for the first time , then lower the temperature to -5 ~ 0 ° C, add 55% TPC for the second time to react for 30 minutes, transfer the reaction mixture to a neutralization tank and add 12% NaOH solution for neutralization to neutrality, and then use deionized water for classification Washing 10 times, steam drying at 140°C to obtain PPTA with a water content of less than 70ppm and an intrinsic viscosity of 7.5-8.5dL / g;

[0031] (2) Preparation of spinning stock solution: at a temperature of 80-100°C, multi-stage jacket temperature control, under nitrogen sealing, mix and stir PPTA with an...

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Abstract

The invention provides a preparation method for a high-modulus para-aramid fiber. The preparation method comprises the following steps: adopting a low-temperature polycondensation method to prepare poly(terephthaloyl-p-phenylene diamine) (PPTA) polymer with intrinsic viscosity of 7.5-8.5dL / g; utilizing high-concentration sulfuric acid for dissolving the polymer to prepare a spinning solution, obtaining fiber tow through a dye-spraying wet-spinning method; and obtaining the high-modulus para-aramid fiber through processes such as washing, neutralizing, washing, drying, oil-applying and winding,wherein modulus of the PPTA fiber is 850-1000g / D, and intrinsic viscosity is 7.0-8.0 dL / g. The high-modulus para-aramid fiber prepared by the method has high strength, high modulus, small degradation, high crystal-degree loss, fewer broken filaments, excellent mechanical property, short drying time and low energy consumption. Drying equipment domestication replaces import, so that technical locking of the drying equipment is broken through, and therefore, industrial development speed is increased.

Description

technical field [0001] The invention relates to the technical field of polymer material synthesis, in particular to a preparation method of high modulus para-aramid fiber. Background technique [0002] High modulus para-aramid fiber is a high-performance fiber material made of PPD and TPC in NMP / CaCl 2 Low-temperature condensation polymerization in the solvent system, the formation of HCl in the reaction process requires alkali metal salts for neutralization, the synthesized PPTA resin is usually washed with water to remove residual solvents and salts, and dried to remove water; PPTA is dissolved in sulfuric acid The liquid crystal solution is prepared in the liquid crystal solution, and the fiber tow is obtained through dry jet wet spinning technology; the fiber tow is washed with water, neutralized, and washed to remove sulfuric acid in the fiber, and then high-modulus fiber is obtained through high-temperature setting. Because of its excellent mechanical properties, it i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/90D01F1/10D01D10/06D01D5/06D01D1/06C08G69/32
CPCD01F6/905D01F1/10D01D5/06D01D1/065D01D10/06C08G69/32
Inventor 唐凯侯春蕾季先恒于宏广杨文华
Owner 宁夏泰和芳纶纤维有限责任公司
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