Method for preparing heterocyclic aramid solution

A heterocyclic aramid solution technology, which is applied in the field of preparation of heterocyclic aramid solution, can solve the problems of reducing fiber mechanical properties, fiber mechanical properties, and increasing costs, and achieves reduced corrosion, fewer holes and impurities, and better mechanical properties. high effect

Inactive Publication Date: 2017-05-24
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The addition of inorganic salt will bring several disadvantages. The first is to increase the cost, including the cost of the inorganic salt itself, the energy consumption of washing the inorganic salt in the later stage and the increased process cost of recycling the inorganic salt, etc.; the second is that the inorganic salt will affect the equipment. cause some corrosion
Third, when the inorganic salt diffuses from the inside of the fiber macromolecular chain to the outside during the coagulation process and the washing process, some holes will inevitably be left, which will lead to a decline in the mechanical properties of the fiber; In the process, it will also reduce the mechanical properties of the fiber

Method used

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  • Method for preparing heterocyclic aramid solution
  • Method for preparing heterocyclic aramid solution
  • Method for preparing heterocyclic aramid solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 160 grams of PABZ was added to 7.0 L of HMPA solvent, wherein the water content in the solvent was 300 ppm. Then 77.14 g of PDA was added, stirred under the protection of nitrogen until the diamine was dissolved, and then the temperature was lowered to 0°C. Then add 232 grams of TPC (80% of the total amount of TPC) to react for 20 minutes, then raise the reaction temperature to 30°C, then add the remaining TPC and stir for 1 hour to obtain a viscous heterocyclic aramid solution, wherein the ratio of mole fraction to TPC :PABZ:PDA=10:5:5, the solid content of heterocyclic aramid fiber is 5.0%.

[0043] The obtained heterocyclic aramid fiber solution is prepared by conventional wet spinning to prepare raw yarns, and static heat treatment is performed at 360° C. to obtain finished heterocyclic aramid fiber yarns. And carry out solvent recovery to the whole process, the solvent recovery rate is 97%. Ubbelohde viscometer was used to test the intrinsic viscosity of the hete...

Embodiment 2

[0045] The HMPA solvent recovered in Example 1 was subjected to polymerization again. 155.2 grams of PABZ was added to 6.79 L of recovered HMPA solvent, wherein the moisture content in the solvent was controlled to be 300 ppm. Then 74.82 g of PDA was added, stirred under the protection of nitrogen until the diamine was dissolved, and then the temperature was lowered to 0°C. Then add 225.04 grams of TPC (80% of the total amount of TPC) to react for 20 minutes, then raise the reaction temperature to 30°C, then add the remaining TPC and stir for 1 hour to obtain a viscous heterocyclic aramid solution, wherein the ratio of mole fraction TPC:PABZ:PDA=10:5:5, the solid content of heterocyclic aramid fiber is 5.0%.

[0046] The obtained heterocyclic aramid fiber solution is prepared by conventional wet spinning to prepare raw yarns, and static heat treatment is performed at 360° C. to obtain finished heterocyclic aramid fiber yarns. And carry out solvent recovery to the whole proce...

Embodiment 3

[0048] Polymerization was carried out according to the method of Example 1, wherein TPC:PABZ:PDA=10:7:3, the solid content of the heterocyclic aramid fiber was 5.5%, and the moisture content in the solvent HMPA was 200ppm. Under the protection of argon, two diamines, PABZ and PDA, were first added to the solvent HMDA. After the diamines were dissolved, the temperature was lowered to -10°C. Then add 90% TPC and react for 30 minutes, then raise the reaction temperature to 20°C, then add the rest of TPC and stir for 0.5h to get a viscous heterocyclic aramid solution.

[0049] The obtained heterocyclic aramid fiber solution was prepared by conventional wet spinning to prepare raw yarns, and static heat treatment was performed at 380° C. to obtain finished heterocyclic aramid fiber yarns. And carry out solvent recovery to the whole process, the solvent recovery rate is 98%. Ubbelohde viscometer was used to test the intrinsic viscosity of the heterocyclic aramid fiber, and the resu...

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Abstract

The invention belongs to the technical fields of heterocyclic aramid solution and preparation thereof, and specifically, relates to a method for preparing a heterocyclic aramid solution, wherein the method comprises the steps: a diamine substance and an aromatic dicarbonyl chloride are subjected to a polymerization reaction in an inert gas atmosphere and in a hexamethylphosphoric triamide solution containing no cosolvent, wherein the diamine substance comprises 2-(4-aminophenyl)-5-aminobenzimidazole.

Description

technical field [0001] The invention belongs to the technical field of heterocyclic aramid solution and its preparation, and in particular relates to a preparation method of heterocyclic aramid solution. Background technique [0002] Heterocyclic aramid fibers are high-strength and 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 spinning to obtain high-stren...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32C08G69/28D01F6/60D01F6/80D01F13/04
CPCC08G69/28C08G69/32D01F6/605D01F6/805D01F13/04Y02P70/62
Inventor 刘向阳戴宇侯庆华罗龙波王旭刘昌莉
Owner SICHUAN UNIV
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