Method for preparing poly(p-phenylene terephthalamide)

A technology for poly-p-phenylene terephthalamide and terephthaloyl chloride is applied in the field of preparing poly-p-phenylene terephthalamide polymers, and can solve the problem of removal, strong exothermic removal, and reaction heat removal. and other problems, to achieve the effect of uniform temperature, uniform local temperature, and increased molecular weight

Inactive Publication Date: 2011-08-31
北京国能新兴化工科技发展有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the problem that a large amount of heat of reaction cannot be removed in time in the large-scale continuous preparation process of poly-p-phenylene terephthalamide, and provides a method for preparing poly-p-phenylene terephthalamide polymer. To make up for the deficiencies or defects of the existing technology and meet the needs of production
[0006] A method for preparing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] When equipped with a strong stirring device, N 2 In the 140L reactor at the inlet and outlet, feed the dry high-purity N first. 2 The air in the reactor was replaced. in N 2 Under protection, add 30L solvent and 1000g co-solvent successively, stir and dissolve at 50°C and cool to room temperature, wherein the solvent is N-methylpyrrolidone (NMP), and the co-solvent is calcium chloride, while stirring, add p-phenylenediamine ( PPD) powder 1580g, stirring and dissolving at room temperature. When the system is cooled to -10°C, add 1.5L of pyridine as an additive, 1485g of terephthaloyl chloride (TPC) and 3L of liquid nitrogen, and increase the stirring speed at the same time, 200rpm can be selected, and then add 1485g of TPC after reacting for 10 to 20 minutes. Phthaloyl chloride (TPC) and 3L liquid nitrogen, after the system appears gel, continue to stir rapidly for 20 minutes, the stirring speed can be 400rpm, and the gel block is beaten into powder.

[0026] The pol...

Embodiment 2

[0029] In addition to the complete dissolution of the co-solvent powder in the solvent, the method of adding liquid nitrogen to the system is used to rapidly cool the solvent / co-solvent system to 10-25°C, and the mass ratio of the amount of liquid nitrogen added to the amount of solvent added is 1:20 Outside, all the other are identical with embodiment 1.

Embodiment 3

[0031] When equipped with a strong stirring device, N 2 In the 140L reactor at the inlet and outlet, feed the dry high-purity N first. 2 The air in the reactor was replaced. in N 2 Under protection, add 30L solvent and 1500g co-solvent in turn, stir and dissolve at 50°C and cool to room temperature. The co-solvent powder is dissolved in the solvent overshoot, and the system maintains a slight positive pressure. The solvent is dimethylacetamide, and the co-solvent is chlorine. Lithium oxide. While stirring, 1296 g of p-phenylenediamine (PPD) powder was added, and stirred and dissolved at room temperature. When the system is cooled to 0°C, add 2L of α-picoline as an additive, 1218g of terephthaloyl chloride (TPC) and 2.5L of liquid nitrogen, and increase the stirring speed at the same time. Add 1218g of terephthaloyl chloride (TPC) and 2.5L of liquid nitrogen, and continue to stir rapidly for 20 minutes after the system gels. The stirring speed can be selected as 700rpm, and...

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Abstract

The invention discloses a method for preparing poly(p-phenylene terephthalamide) (PPTA) in the technical field of the preparation of PPTA. In the method, p-phenylenediamine and terephthaloyl dichloride are used as polymer monomers; and liquid nitrogen is added in the polymerization process to solve the problem of removing the reaction heat. By analyzing the coupling of the polymerization process of PPTA, the direct transition heat-removing technology is utilized to solve the problem of removing a large quantity of released heat in the polymerization process, thus the overall temperature of the reactor can be uniform and the local temperature in the reactor can be uniform. By adopting the process coupling method, the entire polymerization process of PPTA tends to be milder, the heat transfer problem of the polymerization process of PPTA can be solved, the oxidation of monomer caused by the reaction heat of the polymerization process can be effectively improved and the molecular weight of the polymer can be fully increased. The entire polymerization process can be simple and practical and engineering scale-up is easy to perform.

Description

technical field [0001] The invention belongs to the technical field of preparation of polyparaphenylene terephthalamide (PPTA), in particular to a method for preparing polyparaphenylene terephthalamide polymer. Background technique [0002] Polyparaphenylene terephthalamide (PPTA for short) is a high-tech fiber prepared by liquid crystal spinning technology. It has high strength, high modulus, high temperature resistance, chemical corrosion resistance, good wear resistance, light density, Dimensional stability and a series of excellent properties. Therefore, PPTA has important application value in many fields such as aerospace industry, national defense industry, transportation, high temperature protection, composite materials and sports equipment, and has become one of the fastest-growing high-performance fibers for industrial fiber materials. [0003] However, with the continuous deepening of the research on the PPTA polymerization process, we found that the control of th...

Claims

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Application Information

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IPC IPC(8): C08G69/32C08G69/28
Inventor 魏飞罗国华张涛卢俨俨徐宁力骞伟中庹新林王晓工张楠
Owner 北京国能新兴化工科技发展有限公司
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