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A method for preparing heterocyclic aramid fiber based on chain extension reaction after high temperature

A technology of heterocyclic aramid and post-chain extension, which is applied in the field of preparation of heterocyclic aramid fiber by high-temperature post-chain extension reaction, can solve the problems of increasing the production cost of heterocyclic aramid fiber and increasing the preparation process, and achieve the reduction of solvent recovery cost, The effect of increasing solid content and high molecular weight

Active Publication Date: 2018-12-14
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the preparation process of the heterocyclic aramid fiber can increase the solid content of the spinning solution, it will obviously increase the preparation process, and finally increase the production cost of the heterocyclic aramid fiber

Method used

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  • A method for preparing heterocyclic aramid fiber based on chain extension reaction after high temperature
  • A method for preparing heterocyclic aramid fiber based on chain extension reaction after high temperature
  • A method for preparing heterocyclic aramid fiber based on chain extension reaction after high temperature

Examples

Experimental program
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Effect test

Embodiment 1

[0077] Under a nitrogen atmosphere, 169 g of PABZ was added to 5 L of DMAC / LiCl solvent with a water content of 150 ppm. Then add 82g of PDA, stir until the diamine is dissolved, and lower the temperature to 0°C. Then add 300gTPC, heat up to 30°C after reacting for 20min, and continue stirring for 1h to obtain an amino-terminated aramid solution, wherein the mole fraction ratio is TPC:PABZ:PDA=98:50:50, and the solid content of the heterocyclic aramid is 8%. Also under a nitrogen atmosphere, 305 g of TPC was added to 5 L of DMAC / LiCl with a water content of 150 ppm, and the temperature of the solution was lowered to 0°C. Then add 165g PABZ and 80g PDA, react for 20 minutes, raise the temperature to 30°C, and continue the reaction for 1 hour to obtain an acid chloride-terminated aramid solution, and finally add distilled water in an equimolar ratio of the residual acid chloride end groups. Wherein the mole fraction ratio is TPC:PABZ:PDA=100:49:49, and the solid content of the...

Embodiment 2

[0080] Under a nitrogen atmosphere, 237 g of PABZ was added to 5 L of DMAC / LiCl solvent with a water content of 100 ppm. Then add 49g of PDA, stir until the diamine is dissolved, and lower the temperature to 0°C. Then add 300gTPC, heat up to 30°C after reacting for 20min, and continue to stir for 1h to obtain an amino-terminated aramid solution, wherein the mole fraction ratio is TPC:PABZ:PDA=98:70:30, and the solid content of the heterocyclic aramid is 8%. Also under a nitrogen atmosphere, 305 g of TPC was added to 5 L of DMAC / LiCl with a water content of 100 ppm, and the temperature of the solution was lowered to 0°C. Then add 165gPABZ and 80gPDA, after 20min of reaction, raise the temperature to 30°C, continue the reaction for 1h to obtain the aramid fiber solution capped by acid chloride, and finally add distilled water according to the equimolar ratio of residual acid chloride end groups, wherein the mole fraction ratio is TPC:PABZ: PDA=100:69:29, the solid content of t...

Embodiment 3

[0083] Polymerization is carried out according to the method of Example 1, wherein in the amine-terminated solution TPC:PABZ:PDA=98:100:0, the water content is 200ppm, first add diamine monomer, after the diamine monomer dissolves, the solution temperature Lower the temperature to 0°C, add acid chloride, react for 30 minutes, then raise the temperature to 30°C, and continue the reaction for 1 hour to obtain an amino-terminated aramid fiber solution. In the acid chloride-capped solution, TPC:PABZ:PDA=100:98:0, the water content is 200ppm, add the acid chloride first, cool down to 0°C after the acid chloride dissolves, add the diamine monomer to react for 30min, then raise the temperature to 30°C to continue the reaction 1h to obtain the heterocyclic aramid fiber solution terminated by acid chloride, and finally add distilled water according to the equimolar ratio of residual acid chloride end groups. The solid content of the two heterocyclic aramid solutions is 8%. The two sol...

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Abstract

The invention provides a method for preparing heterocyclic aramid fibers based on chain extension reaction after high temperature, mainly based on the characteristics that amino groups and carboxyl groups do not undergo chemical reactions at low temperatures, so that amino-terminated oligomers with lower dynamic viscosity and The carboxyl-terminated oligomer does not undergo condensation reaction in the blending and spinning stages, so that it can maintain low dynamic viscosity at higher solid content; at the same time, condensation reaction can occur at high temperature (≥200°C) based on amino and carboxyl groups The characteristics of the heterocyclic aramid fiber make it undergo a condensation reaction in the high-temperature post-treatment process stage required by the heterocyclic aramid itself, thereby realizing macromolecular chain extension and obtaining a finished heterocyclic aramid yarn with a higher molecular weight. Compared with the heterocyclic aramid prepared by the traditional method, the intrinsic viscosity is higher, which can be as high as 12-14dL / g; the tensile strength is higher, which can reach 26-31cN / dt; the initial modulus is larger, which can reach 880-1100cN / dt. The molecular weight is also higher.

Description

technical field [0001] The invention relates to the technical field of preparation of heterocyclic aramid fiber, in particular to a method for preparing heterocyclic aramid fiber based on high-temperature post-chain extension reaction. Background technique [0002] Heterocyclic aramid fibers are high-strength, high-modulus organic fibers, and their mechanical properties and composite properties with resins are higher than those of traditional aramid II fibers (Kevlar fibers from DuPont). It has been widely used in the fields of bulletproof products, special protective clothing and electronic equipment, and its composite materials with resins have also been used in aerospace, national defense and military industries. The traditional heterocyclic aramid fiber is obtained by solution polycondensation of terephthaloyl dichloride, p-phenylenediamine and its third monomer (2-(4-aminophenyl)-5-aminobenzimidazole). Aramid solution, and then heat treatment / heat stretching after wet ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/60C08G69/32
CPCC08G69/32D01F6/605
Inventor 刘向阳戴宇罗龙波侯庆华程政王旭刘昌莉
Owner SICHUAN UNIV