Self-flowing meta-aramid and preparation method thereof

A self-flowing, aramid fiber technology, applied in the direction of single-component polyamide rayon, etc., can solve the problems that the solubility of meta-aramid fibers cannot be improved, and the processing performance has not been improved, so as to achieve excellent self-flowing performance and excellent flow Performance, effect of widening spinning conditions

Active Publication Date: 2014-05-14
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 these methods cannot improve the solubility of meta-aramid fibers, so the processing performance has not been improved.

Method used

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  • Self-flowing meta-aramid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 5.0g of 2,4-diaminobenzenesulfonic acid (2,4-DABSA) with a purity greater than 97% and 20ml of dimethylacetamide (DMAC) into a 250ml four-neck flask, then add to dissolve 2.35 g of anhydrous LiCl in 80 ml of DMAC, then stirred at 100 °C until homogeneous. 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 it dropwise to a four-neck flask. When the exotherm ceased, the ice bath was removed and stirred at room temperature for 24 hours. Take by weighing 1.11g NaOH again and add in the solution, stir 3 hours, then add the 30g Jimine quaternary ammonium salt NPEQ (C 9 h 19 C 6 h 4 (OCH 2 CH 2 ) 10 O(CH 2 ) 2 N + (CH 3 ) 3 Cl - ), stirred rapidly for 6 hours, poured the final liquid into a dialysis bag, and dialyzed in the presence of circulating water, then placed the sample in the d...

Embodiment 2

[0028] Weigh 5.0g of 2,4-diaminobenzenesulfonic acid (2,4-DABSA) with a purity greater than 97% and 20ml of N-methylpyrrolidone at room temperature and pour them into a 250ml four-neck flask, then add and dissolve in 4.00 g of anhydrous CaCl in 70 ml of N-methylpyrrolidone 2 , and then stirred at 90°C until homogeneous. Then add 5.4g of isophthaloyl chloride (ICI) dissolved in 30ml of N-methylpyrrolidone to the constant pressure funnel, then lower the reaction temperature to 2°C, make TPC under nitrogen flow and rapid stirring within 5-6 minutes Added dropwise to a four-neck flask under certain conditions. When the exotherm ceased, the ice bath was removed and stirred at room temperature for 24 hours. Then weigh 1.11g NaOH and add it to the solution, stir for 3 hours, then add 20g C dissolved in 200ml distilled water to the four-necked flask. 6 h 13 C 6 h 4 (OCH 2 CH 2 ) 8 O(CH 2 ) 2 N + (CH 3 ) 3 Cl -, stirred rapidly for 7 hours, poured the final liquid into a...

Embodiment 3

[0030] Weigh 10.0g of 2,4-diaminobenzenesulfonic acid (2,4-DABSA) with a purity greater than 97% and 10ml of N-methylpyrrolidone at room temperature and pour them into a 250ml four-neck flask, then add and dissolve in 80ml of N-methylpyrrolidone in 5g of anhydrous LiCl, then stirred at 80°C until homogeneous. Add 11 g of isophthaloyl chloride (ICI) dissolved in 30 ml of N-methylpyrrolidone to the constant pressure funnel, then reduce the reaction temperature, and make the TPC under nitrogen flow and rapid stirring within 3-5 minutes Add it dropwise to a four-neck flask. When the exotherm ceased, the ice bath was removed and stirred overnight at room temperature. Then weigh 3.11g KOH and add it to the solution, stir for 3 hours, then add 21g (CH) dissolved in 200ml distilled water to the four-necked flask 3 O) 3 Si(CH 2 ) 5 N + (CH 3 )(C 10 h 21 )Cl - , stirred rapidly for 5 hours, poured the final liquid into a dialysis bag, dialyzed in the presence of circulating wa...

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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 fla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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