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Method for preparing high molecular weight poly(p-phenyleneterephthalamide) and products

A technology of poly-p-phenylene terephthalamide and p-phenylene phthalamide, which is applied in the field of raw material preparation in the process of aramid fiber spinning, and can solve the problem of poly-p-phenylene terephthalamide Molecular weight, large amount of calcium chloride, difficult to control and other problems, to achieve the effect of high molecular weight, good color, and reduced side reactions

Active Publication Date: 2009-06-17
YANTAI TAYHO ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amount of calcium chloride is large, and the reaction temperature can exceed 100°C, which is difficult to control, and there are many side reactions, which affect the molecular weight of poly-p-phenylene terephthalamide (PPTA).

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A kind of preparation method of high molecular weight polyparaphenylene terephthalamide (PPTA), comprises the following steps:

[0016] (1) Add 3.5Kg of anhydrous calcium chloride, 80Kg of N-methylpyrrolidone (NMP), and 3.45Kg of p-phenylenediamine (PPD) into the reactor, start stirring, and stir at room temperature for 30 minutes;

[0017] (2) The jacket of the reactor is cooled with a refrigerant to lower the temperature of the system to 0~-15°C, add the first batch of terephthaloyl chloride (TPC) 1.3Kg, and continue to stir for 30 minutes;

[0018] (3) Lower the temperature to 0~-15°C, add the second batch of TPC5.2Kg, and stir rapidly. After the reaction system appears gel, climbs rods, and is crushed again, stop the reaction to obtain polyterephthaloyl para Phenylenediamine (PPTA).

[0019] The poly-p-phenylene terephthalamide (PPTA) prepared according to the method has an intrinsic viscosity of more than 6.0 and a molecular weight of more than 20,000. It can be ...

Embodiment 2

[0021] A kind of preparation method of high molecular weight polyparaphenylene terephthalamide (PPTA), comprises the following steps:

[0022] (1) Add 4Kg of anhydrous calcium chloride, 100Kg of N-methylpyrrolidone (NMP), and 3.45Kg of p-phenylenediamine (PPD) into the reactor, start stirring, and stir at room temperature for 30 minutes;

[0023] (2) The jacket of the reactor is cooled with a refrigerant to lower the temperature of the system to 0~-15°C, add the first batch of terephthaloyl chloride (TPC) 1.3Kg, and continue to stir for 30 minutes;

[0024] (3) Lower the temperature to 0~-15°C, add the second batch of TPC5.2Kg, and stir rapidly. After the reaction system appears gel, climbs rods, and is crushed again, stop the reaction to obtain polyterephthaloyl para Phenylenediamine (PPTA).

[0025] The poly-p-phenylene terephthalamide (PPTA) prepared according to the method has an intrinsic viscosity of more than 6.0 and a molecular weight of more than 20,000. It can be w...

Embodiment 3

[0027] A kind of preparation method of high molecular weight polyparaphenylene terephthalamide (PPTA), comprises the following steps:

[0028] (1) Add 20Kg of anhydrous calcium chloride, 100Kg of N-methylpyrrolidone (NMP), and 3.45Kg of p-phenylenediamine (PPD) into the reactor, start stirring, and stir at room temperature for 30 minutes;

[0029] (2) The jacket of the reactor is cooled with a refrigerant to lower the temperature of the system to 0~-15°C, add the first batch of terephthaloyl chloride (TPC) 1.3Kg, and continue to stir for 30 minutes;

[0030] (3) Then lower the temperature to 0~-15°C, add the second batch of TPC 5.2Kg, and stir rapidly. After the reaction system appears gel, climbs rods, and is crushed again, stop the reaction to obtain terephthaloyl-p-phenylene diamine.

[0031] The poly-p-phenylene terephthalamide (PPTA) prepared according to the method has an intrinsic viscosity of more than 6.0 and a molecular weight of more than 20,000. It can be widely ...

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PUM

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Abstract

A preparation method for the p-phenylene terephthalamide p-phenylenediamine with high molecular weight, which comprises the following steps: adding anhydrous calcium chloride and N-methylpyrrolidone (NMP) to a reactor according to the weight proportion of 4-20: 100; adding proper amount of p-phenylenediamine (PPD), starting stirring, stirring for 30min at room temperature; inletting cooling medium to the reactor jacket to reduce temperature; reducing the system temperature to 0-15 DEG C below zero; adding the first batch of terephthaloyl chloride (TPC), continually stirring for 30min; reducing the temperature to 0-15 DEG C below zero again; adding the second batch of TPC; stirring quickly; stopping reaction after the system occurs pole-climbing and gel and is stirred to prepare the p-phenylene terephthalamide p-phenylenediamine. By adding the reactant TPC by two batches, the method of the invention can effectively control the reaction temperature; by cooling and reducing the temperature of the system, the method reduces the occurrence of side reaction and prepares the p-phenylene terephthalamide p-phenylenediamine with higher molecular weight and better color and luster.

Description

technical field [0001] The invention relates to a method for preparing raw materials in the spinning process of aramid fibers, in particular to a method for preparing high-molecular-weight polyparaphenylene terephthalamide (PPTA) and a product thereof. Background technique [0002] PPTA-type aramid is made of poly-p-phenylene terephthalamide (PPTA) spinning, and the main products are DuPont's Teijin's Wait. The most outstanding properties of para-aramid are its high strength, high modulus and excellent heat resistance. At the same time, it also has appropriate toughness for textile processing. The weight ratio of standard PPTA aramid fiber is 6 times that of steel wire, 3 times that of glass fiber, and 2 times that of high-strength nylon industrial yarn; its tensile modulus is 3 times that of steel wire, 2 times that of glass fiber, and high-strength nylon industry. 10 times that of silk; after 100 hours at 200°C, it can still maintain 75% of the original strength, and...

Claims

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Application Information

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IPC IPC(8): C08G69/32C08G69/28D01F6/60
Inventor 周爱民朱敏英唐凯
Owner YANTAI TAYHO ADVANCED MATERIALS CO LTD
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