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Continuous polymerization method of high-viscosity poly-p-phenylene terephthamide

A technology for poly(p-phenylene terephthalamide) and a polymerization method is applied in the field of polymer synthesis and can solve the problems of large difference in flow rate between PPD solution and TPC melt, unsatisfactory mixing effect, and inability of continuous and stable polymerization production. , to achieve the effect of prolonging the effective polymerization time, stabilizing the continuous polymerization production and improving the stability

Active Publication Date: 2013-04-24
AFCHINA CORP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the relatively large flow difference between PPD solution and TPC melt, the mixing effect in actual use is not ideal
Other simple mixers, such as tube mixers, are often blocked due to the precipitation of PPD and TPC polymers, resulting in continuous and stable polymerization production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Add 450L of solvent N-methylpyrrolidone into a 600L dissolution kettle, and add 45Kg of calcium chloride, a solubilizing salt, under nitrogen protection and stirring, and heat at 100°C to dissolve the solubilizing salt. Then, the temperature of the dissolution tank was lowered to 15° C., and 19.467 Kg of p-phenylenediamine was added under stirring for dissolution. The molar concentration of p-phenylenediamine in the solvent system was 0.4 mol / L. Then cool down the dissolution tank to 0°C, meter it through the transfer pump and flowmeter and transfer it to the mixer; the terephthaloyl chloride melt at 90°C is also metered and transferred to the mixer through the transfer pump and flowmeter center nozzle.

[0020] (2) The terephthaloyl chloride melt is sprayed from the central nozzle of the mixer, and mixed with the p-phenylenediamine solution sprayed from the annular jet port of the mixer, and the molar ratio of TPC and PPD is controlled by accurate metering as TPC:P...

Embodiment 2

[0023] (1) Add 450L of solvent N-methylpyrrolidone into a 600L dissolution kettle, and add 40Kg of calcium chloride, a solubilizing salt, under nitrogen protection and stirring, and heat at 100°C to dissolve the solubilizing salt. Then, the temperature of the dissolution tank was lowered to 15° C., and 24.332 Kg of p-phenylenediamine was added under stirring for dissolution. The molar concentration of p-phenylenediamine in the solvent system was 0.5 mol / L. Then cool down the dissolution tank to 0°C, meter it through the transfer pump and flowmeter and transfer it to the mixer; the terephthaloyl chloride melt at 90°C is also metered and transferred to the mixer through the transfer pump and flowmeter center nozzle.

[0024] (2) The terephthaloyl chloride melt is sprayed from the center nozzle of the mixer, and mixed with the p-phenylenediamine solution sprayed from the annular jet port of the mixer. The added molar ratio of TPC and PPD is controlled by accurate metering to be ...

Embodiment 3

[0027] (1) Add 450L of solvent N-methylpyrrolidone into a 600L dissolution kettle, and add 38Kg of calcium chloride, a solubilizing salt, under nitrogen protection and stirring, and heat at 90°C to dissolve the solubilizing salt. Then the temperature of the dissolution tank was lowered to 20° C., and 24.332 Kg of p-phenylenediamine was added under stirring for dissolution. The molar concentration of p-phenylenediamine in the solvent system was 0.5 mol / L. Then cool down the dissolution tank to -5°C, and meter it through the transfer pump and flowmeter and transfer it to the mixer; the terephthaloyl chloride melt at 85°C is also metered and transferred to the mixer through the transfer pump and flow meter. Mixer center nozzle.

[0028] (2) The terephthaloyl chloride melt is sprayed from the center nozzle of the mixer, and mixed with the p-phenylenediamine solution sprayed from the annular jet port of the mixer. The added molar ratio of TPC and PPD is controlled by accurate mete...

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PUM

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Abstract

The invention provides a continuous polymerization method of high-viscosity poly-p-phenylene terephthamide. Based on the design of the polymerization formula, and the design and use of a novel mixing device and a hydrogen chloride discharge device matched with the design of the polymerization formula, continuity of the PPTA (poly-p-phenylene terephthamide) polymerization is guaranteed, and the molecular weight of the obtained PPTA is high. The method is characterized by comprising the following steps of: preparing materials, namely dissolving hydrotropy salt and PPD (p-Phenylenediamine) at a low temperature; keeping the TPC (paraphthaloyl chloride) in molten state; mixing, by combination of a Venturi jet mixer and a dynamic or static mixer, ensuring even mixing of the TCP and the PPD solution; and polymerization, finishing the polymerization of the PPD and the TPC by a double-screw reactor, and eliminating the hydrogen chloride released by some reaction. The continuous polymerization method has the advantages of improving the stability of the PPD and TCP reaction, ensuring the continuity and the stability of the production, and facilitating the high-efficiency separation of the hydrogen chloride; by the continuous polymerization method provided by the invention, polymerization production of high-viscosity PPTA can be realized steadily and continuously.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a continuous polymerization method of high-viscosity poly-p-phenylene terephthalamide. Background technique [0002] Poly(p-phenylene terephthalamide) (hereinafter referred to as PPTA) fiber is a high-strength and high-modulus fiber with many excellent properties such as high strength, high modulus, high temperature resistance and solvent resistance, and is used in aerospace, national defense and many civil applications. There are important applications in the field. Stable mass production of high-viscosity PPTA resin is a prerequisite for the production of PPTA fibers. The commonly used PPTA polymerization method is the low temperature solution polycondensation method. This method uses terephthaloyl dichloride (hereinafter referred to as TPC) and p-phenylenediamine (hereinafter referred to as PPD) as raw materials to react in a suitable solvent system at ...

Claims

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Application Information

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IPC IPC(8): C08G69/32
Inventor 庹新林许甲王晓工崔庆海周凯
Owner AFCHINA CORP CO LTD
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