Self-flowing meta-aramid and preparation method thereof

A self-flowing, aramid fiber technology, applied in the direction of one-component polyamide rayon filament, can solve the problems of inability to improve the solubility of meta-aramid fibers and the processing performance is not improved, and achieve excellent self-flowing performance, excellent flow performance, effect of broadening spinning conditions

Active Publication Date: 2012-10-17
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the above analysis, it can be seen that there are various methods for the synthesis of meta-aramid fibers, but t

Method used

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  • Self-flowing meta-aramid and preparation method thereof

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Example Embodiment

[0026] Example 1

[0027] Weigh 5.0g of 2,4-Diaminobenzenesulfonic acid (2,4-DABSA) with a purity greater than 97% and measure 20ml of dimethylacetamide (DMAC) into a 250ml four-necked flask, and then add to dissolve 2.35g anhydrous LiCl in 80 ml DMAC, then stir at 100°C until homogeneous. Then add 5.4 g of isophthaloyl chloride (ICI) dissolved in 30 ml of DMAC to the constant pressure funnel, then lower the reaction temperature to 0°C, and make the TPC under nitrogen flow and rapid stirring within 3-5 minutes Add dropwise to the four-necked flask. When the heat is no longer exothermic, remove the ice bath and stir at room temperature for 24 hours. Weigh 1.11g NaOH and add it to the solution, stir for 3 hours, and then add 30g gemine quaternary ammonium salt NPEQ dissolved in 200ml distilled water into the four-neck flask (C 9 H 19 C 6 H 4 (OCH 2 CH 2 ) 10 O(CH 2 ) 2 N + (CH 3 ) 3 Cl - ), quickly stir for 6 hours, pour the final liquid into a dialysis bag, dialyze in the prese...

Example Embodiment

[0028] Example 2

[0029] Weigh out 5.0g of 2,4-diaminobenzenesulfonic acid (2,4-DABSA) with a purity of more than 97% and measure 20ml of N-methylpyrrolidone into a 250ml four-necked flask at room temperature, and then add it to dissolve in 70ml N-methylpyrrolidone in 4.00g anhydrous CaCl 2 , And then stir at 90 ℃ until uniform. Then add 5.4g of isophthaloyl chloride (ICI) dissolved in 30ml of N-methylpyrrolidone into the constant pressure funnel, then lower the reaction temperature to 2°C, and make the TPC under nitrogen flow and rapid stirring within 5-6 minutes Add dropwise to a four-necked flask under the conditions of When the heat is no longer exothermic, remove the ice bath and stir at room temperature for 24 hours. Weigh 1.11g NaOH and add it to the solution, stir for 3 hours, then add 20g C dissolved in 200ml distilled water into the four-neck flask 6 H 13 C 6 H 4 (OCH 2 CH 2 ) 8 O(CH 2 ) 2 N + (CH 3 ) 3 Cl - , Quickly stir for 7 hours, pour the final obtained liquid...

Example Embodiment

[0030] Example 3

[0031] Weigh out 10.0g of 2,4-diaminobenzenesulfonic acid (2,4-DABSA) with a purity greater than 97% and 10ml of N-methylpyrrolidone at room temperature into a 250ml four-necked flask, and then add the 80ml N-methylpyrrolidone in 5g anhydrous LiCl, then stir at 80°C until homogeneous. Then add 11 g of isophthaloyl chloride (ICI) dissolved in 30 ml of N-methylpyrrolidone into the constant pressure funnel, then lower the reaction temperature, and make the TPC under nitrogen flow and rapid stirring within 3-5 minutes Add dropwise to the four-necked flask. When the heat is no longer exothermic, remove the ice bath and stir overnight at room temperature. Weigh 3.11g KOH and add it to the solution, stir for 3 hours, and then add 21g (CH 3 O) 3 Si(CH 2 ) 5 N + (CH 3 )(C 10 H 21 )Cl - , Quickly stir for 5 hours, pour the final obtained liquid into a dialysis bag, dialyze in the presence of circulating water, and then place the sample in the dialysis bag in a vacuum...

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Abstract

The invention provides a self-flowing meta-aramid and a preparation method thereof. The preparation method comprises the following steps: 1) dissolving m-phenylenediamine with sulfonic groups and the additive lithium chloride or calcium chloride in a solvent to prepare a solution, maintaining the temperature of the solution to be 80 to 100 DEG C, adding an m-phthalyl dichloride solution, decreasing reaction temperature and adding m-phthalyl dichloride into the solvent of m-phenylenediamine with sulfonic groups under the conditions of inert gas and rapid stirring in 1 to 8 min for a reaction; and 2) adding alkali into the solution obtained in step 1), allowing alkali to react with the solution and adding a quaternary ammonium salt solution for reaction, wherein synthesis reaction is finished after 5 to 7 h, a self-flowing meta-aramid material is obtained, and the self-flowing meta-aramid material has a molecular weight of 2000 to 40000 and a thermal decomposition temperature of 300 to 600 DEG C and can be dissolved in water and most organic solvents. Aramid fibers prepared from the self-flowing meta-aramid material have elongation at break of 2 to 4%, compressive strength of 0.01 to 1.00 GPa, tensile strength of 1000 to 6000 MPa and elastic modulus of 1 to 1.6 MPa. Polymerization in the invention is mild and has good controllability, the structure of quaternary ammonium salt is changed, and dissolving performance of a polymer can be adjusted.

Description

technical field [0001] The invention relates to a self-flowing aromatic polyamide and a synthesis method thereof, in particular to a self-flowing meta-aramid for aramid fibers with excellent mechanical properties and excellent processing performance and a synthesis method thereof, belonging to the field of polymer material synthesis. Background technique [0002] According to its structure, aramid can be divided into para-aramid and meta-aramid. Meta-aramid, namely poly-m-phenyleneisophthalamide (PMIA for short), is also known as aramid 1313 in my country. Polym-phenylene isophthalamide is a regularly arranged zigzag macromolecule, which has been decomposed before melting. The glass transition temperature Tg is 270°C, and no obvious decomposition and carbonization will occur below 350°C. When the temperature exceeds 400°C, the fiber will gradually become brittle, carbonized and decomposed, but no molten droplets will be produced; it will not burn in flames and has good ...

Claims

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Application Information

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IPC IPC(8): C08G69/48C08G69/32C08G69/28D01F6/60
Inventor 赵广辉王钦董丽杰袁野熊传溪
Owner WUHAN UNIV OF TECH
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