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A kind of preparation method of polyparaphenylene terephthalamide polymer

A technology for poly(p-phenylene terephthalamide) and terephthaloyl chloride is applied in the field of preparation of high-molecular polymers, and can solve the problems of difficult uniform mixing, wide molecular weight distribution, darker color and the like, and avoid dispersion. Inhomogeneous, stable reaction process and uniform molecular weight

Active Publication Date: 2021-01-01
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a preparation method of poly(p-phenylene terephthalamide) polymer, which overcomes the color change of p-phenylenediamine in the prior art preparation process when it is stored in a solvent for a long time. deep, the reactivity decreases, and the heat release in the reaction process is relatively concentrated, which is not conducive to the control in the industrial continuous production process; the molten or powdered terephthaloyl chloride added later in the preparation process is difficult to achieve uniform mixing with the prepolymer system. Cause problems such as wide molecular weight distribution and even monomer cooling and solidification blockage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) In a dry system protected by a nitrogen atmosphere, add 100 mL of NMP-CaCl to a three-necked flask 2 solution (7%wt), and 0.04mol of PPDA monomer was added, stirred at room temperature until completely dissolved, and then the reaction device was transferred to a refrigerated circulating bath and cooled to -10°C. After the temperature of the reaction system is stable, add 0.042 mol of TPC monomer, and stir the reaction rapidly. At this time, the viscosity of the system rises sharply. After 5 minutes of reaction, it is basically stable, and a low molecular weight PPTA prepolymer system with an acid chloride group as the end group is obtained. The system is In the state of bright yellow slurry, keep the system at -10°C for later use.

[0031] (2) In a dry system protected by a nitrogen atmosphere, add 100 mL of NMP-CaCl to a three-necked flask 2 solution (7%wt), and 0.042mol of PPDA monomer was added, stirred at room temperature until completely dissolved, and then th...

Embodiment 2

[0035] (1) In a dry system protected by a nitrogen atmosphere, add 100 mL of NMP-CaCl to a three-necked flask 2 solution (7%wt), and 0.04mol of PPDA monomer was added, stirred at room temperature until completely dissolved, and then the reaction device was transferred to a refrigerated circulating bath and cooled to -10°C. After the temperature of the reaction system is stable, add 0.042 mol of TPC monomer, and stir the reaction rapidly. At this time, the viscosity of the system rises sharply. After 5 minutes of reaction, it is basically stable, and a low molecular weight PPTA prepolymer system with an acid chloride group as the end group is obtained. The system is In the state of bright yellow slurry, keep the system at -10°C for later use.

[0036](2) In a dry system protected by a nitrogen atmosphere, add 100 mL of NMP-CaCl to a three-necked flask 2 solution (7%wt), and 0.042mol of PPDA monomer was added, stirred at room temperature until completely dissolved, and then the...

Embodiment 3

[0040] (1) In a dry system protected by a nitrogen atmosphere, add 100 mL of NMP-CaCl to a three-necked flask 2 solution (7%wt), and 0.04mol of PPDA monomer was added, stirred at room temperature until completely dissolved, and then the reaction device was transferred to a refrigerated circulating bath and cooled to -10°C. After the temperature of the reaction system is stable, add 0.042 mol of TPC monomer, and stir the reaction rapidly. At this time, the viscosity of the system rises sharply. After 5 minutes of reaction, it is basically stable, and a low molecular weight PPTA prepolymer system with an acid chloride group as the end group is obtained. The system is In the state of bright yellow slurry, keep the system at -10°C for later use.

[0041] (2) In a dry system protected by a nitrogen atmosphere, add 100 mL of NMP-CaCl to a three-necked flask 2 solution (7%wt), and 0.042mol of PPDA monomer was added, stirred at room temperature until completely dissolved, and then th...

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Abstract

The invention relates to a preparation method of a poly (p-phenylene terephthalamide) polymer, which comprises the following steps: adjusting the molar ratio of p-phenylenediamine PPDA to terephthaloyl chloride TPC reaction monomer to determine the critical non-gel point of the polymerization reaction; preparing two kinds of low molecular weight poly (p-phenylene terephthalamide) polymer systems with amino group and acyl chloride group as terminal groups at critical non-gel point; subjecting the two kinds of polymer systems to second copolymerization to obtain the poly (p-phenylene terephthalamide) polymer with high molecular weight. The invention prepares two kinds of low molecular weight poly (p-phenylene terephthalamide) pre-polymer systems with different terminal groups, and the systems can stably exist for certain time, and the PPTA with high molecular weight and good solubility in concentrated sulfuric acid can be obtained by copolymerization. The reaction process is stable and easy to control, which is conducive to the industrial production of poly (p-phenylene terephthalamide) fiber.

Description

technical field [0001] The invention belongs to the field of high molecular polymer preparation, in particular to a preparation method of poly(p-phenylene terephthalamide) polymer. Background technique [0002] Poly-p-phenylene terephthalamide (PPTA) is the raw material for preparing high-performance fiber para-aramid. It has excellent thermal properties, chemical stability, electrical insulation, and excellent wear resistance. It is currently widely used It is used in aerospace, national defense and military industry, transportation and communication, sports and leisure, rope and optical cable and other fields. The stability, molecular weight and molecular weight distribution of the polymer synthesis process play a decisive role in the quality of para-aramid products. However, the polymerization process of poly-p-phenylene terephthalamide concentrates a large amount of heat release, and the rigidity of the molecular chain is easy to gel precipitation. Therefore, how to opt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/32C08G69/28
CPCC08G69/28C08G69/32
Inventor 胡祖明于俊荣张兴珂王彦诸静
Owner DONGHUA UNIV
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