Self-flowing para-phenylene terephthalamide and preparation method thereof

A para-aramid fiber, self-flowing technology, applied in the direction of single-component polyamide rayon, can solve the problems of inability to improve the solubility of aramid fiber, decline in mechanical properties, deterioration in mechanical properties, etc., and achieve excellent self-flowing performance , the effect of broadening the spinning conditions and smoothing the polymerization reaction

Active Publication Date: 2012-10-03
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Domestic research on aramid fiber mainly focuses on the modification of PPTA, such as modifying PPTA with 1,5-naphthalene diamine, but the addition of 1,5-naphthalene diamine cannot improve the solubility of the copolymer, and the mechanical properties Significantly worse; 3. Introduce substituted p-benzene and m-benzene structures on the polymer main chain, which increases heat resistance and flame retardancy, but also affects the mechanical properties of the fiber; 4. Introduces N substitution on the po...

Method used

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  • Self-flowing para-phenylene terephthalamide and preparation method thereof
  • Self-flowing para-phenylene terephthalamide and preparation method thereof
  • Self-flowing para-phenylene terephthalamide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 5.0g of 2,5-diaminobenzenesulfonic acid (2,5-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. Then add 5.4g terephthaloyl chloride (TPC) dissolved in 30 ml DMAC to the constant pressure funnel, then lower the reaction temperature to 0°C, and make 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 dialysis...

Embodiment 2

[0027] Weigh 5.0g of 2,5-diaminobenzenesulfonic acid (2,5-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 terephthaloyl chloride (TPC) dissolved in 30ml N-methylpyrrolidone to the constant pressure funnel, then lower the reaction temperature to 2°C, and make TPC under nitrogen flow and rapid stirring within 5-6 minutes Added dropwise to a four-neck flask under the condition of 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 + (CH3 ) 3 Cl - , stirred rapidly for 7 hours, poured the final liquid into a dial...

Embodiment 3

[0029] Weigh 10.0g of 2,5-diaminobenzenesulfonic acid (2,5-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. Then add 11g of terephthaloyl chloride (TPC) dissolved in 30 ml of N-methylpyrrolidone to the constant pressure funnel, then lower the reaction temperature, and make 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. 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...

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Abstract

The invention relates to self-flowing para-phenylene terephthalamide and a preparation method thereof. The preparation method comprises the following steps of: 1) dissolving p-phenylenediamine with a sulfonic acid group and lithium chloride or calcium chloride serving as an additive in a solvent to prepare a solution, keeping the temperature of the solution between 80 and 100 DEG C, adding a paraphthaloyl chloride solution into a constant pressure funnel, reducing reaction temperature for 1 to 8 minutes, and adding paraphthaloyl chloride into the solvent containing the p-phenylenediamine for reacting with quick stirring in the presence of inert gases; and 2), adding alkali into the solution for reacting, adding a quaternary ammonium salt solution for reacting, and performing synthetic reaction for 5 to 7 hours to obtain the self-flowing para-phenylene terephthalamide, wherein molecular weight is 2,000 to 40,000, the temperature of thermal decomposition is 400 to 600 DEG C, and the self-flowing para-phenylene terephthalamide can be dissolved in water and most organic solvents. According to aramid fibers prepared from the self-flowing para-phenylene terephthalamide, the break elongation is 2 to 4 percent, the compression strength is 0.02 to 1.29 GPa, the tensile strength is 1,000 to 6,000 MPa, and the modulus of elasticity is 1 to 1.6 Mpa. The method is mild in polymerization reaction and high in controllability; and a structure of quaternary ammonium salt is changed, and the dissolution performance of a polymer can be regulated.

Description

technical field [0001] The invention relates to a self-flowing aromatic polyamide and a synthesis method thereof, in particular to a self-flowing para-aramid for aramid fiber 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. Para-aramid fiber, that is, poly-p-phenylene terephthalamide fiber (para-phenylene terephthalamide, PPTA for short), is also called aramid fiber 1414 in my country. PPTA is a high-tech fiber. Because of its excellent properties such as high strength and high modulus, heat resistance, chemical corrosion resistance, light density and stable size, it is widely used in aerospace industry, automobile industry, IT industry, national defense industry, reinforced concrete and composite materials. It has a wide range of applications in many ...

Claims

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Application Information

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IPC IPC(8): C08G69/48C08G69/32C08G69/28D01F6/60
Inventor 董丽杰王钦邓素芬张俊俊李琦谈太奇熊传溪
Owner WUHAN UNIV OF TECH
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