Polymerization method capable of effectively controlling phase transformation in PPTA (poly-p-phenylene terephthamide) synthesis process

A technology of synthesis process and polymerization method, applied in the direction of single-component copolyamide artificial filament, etc., can solve the problems of large comonomers, damage to system regularity, large monomers, etc., and achieve increased toughness and elongation at break , It is beneficial to mechanical properties and increases the effect of lateral action

Inactive Publication Date: 2013-12-25
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese Patent No. CN101851809A The content of comonomer added in this patent is relatively large, and the molar ratio of comonomer to p-phenylenediamine is 30-100mol%. The amount of addition will change the mechanism of comonomer after entering the system. After a large amount of comonomer enters the system, it seriously damages the regularity of the system. The solvent is easy to diffuse into the molecular chain, but at the same time, its own properties also have a great impact on the system. PPTA resin itself is a relatively rigid molecular chain. A large number of comonomers will destroy this system, resulting in a large drop in mechanical properties
[0004] Chinese Patent No. CN102070781A This patent uses four monomers for copolymerization, introduces 4,4'-diaminodiphenyl ether or 4,4'-diaminodiphenyl sulfide as the third monomer, and introduces m-phenylene Diformyl chloride is the fourth monomer, so the whole polymerization process will be relatively complicated, and the amount of monomer introduced in this patent is relatively large, which will also seriously damage the previous polyterephthaloyl terephthalate Amine system, so the performance will be greatly affected

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023]A polymerization method for controlling phase transition during the synthesis of PPTA. Under the condition of nitrogen atmosphere protection, first dissolve 3g of LiCl in 300ml of NMP (the concentration of LiCl is 10g / L), stir evenly, and then add 0.12g3 , 4'-ODA, 3ml acid absorbent pyridine (concentration of pyridine is 10ml / L), stir until fully dissolved and mixed evenly, then add 6.42gPPD (total concentration of PPD and 3,4'-ODA is 0.2mol / L , the molar ratio of PPD to 3,4'-ODA is 99:1), stirred until completely dissolved, and then passed through a condensation bath at -5°C. After passing through, TPC was added in three times, adding 4.06g each time (the total concentration of TPC 0.2mol / L), stir it to make it fully react, increase the speed to 3000r / min at this time, remove the condensed oil bath when the rod climbing phenomenon occurs, and continue the reaction at room temperature. After the reaction is completed, the improved The inherent viscosity of PPTA resin is ...

Embodiment 2

[0025] A kind of polymerization method of controlling phase transition in the synthetic process of PPTA, under the condition of nitrogen atmosphere protection, first dissolve 9g of LiCl in 300mlNMP (the concentration of LiCl is 30g / L), stir evenly, after making it fully dissolved, add 1.5g4 , 4'-ODA, 9ml acid absorbent pyridine (concentration of pyridine is 30ml / L), stir until fully dissolved and mixed evenly, then add 15.4gPPD (total concentration of PPD and 4,4'-ODA is 0.5mol / L , the molar ratio of PPD to 4,4'-ODA is 95:5), stirred until completely dissolved, and then passed through a condensation bath at -5°C. After passing through, TPC was added in three times, adding 10.15g each time (the total concentration of TPC 0.5mol / L), stir it to make it react fully, increase the rotation speed to 3000r / min at this time, remove the condensed oil bath when the rod climbing phenomenon occurs, and continue the reaction at room temperature. After the reaction is completed, the improved ...

Embodiment 3

[0027] A kind of polymerization method of controlling phase transition in the synthetic process of PPTA, under nitrogen atmosphere protection condition, first dissolve the LiCl of 4.8g in 300mlNMP (the concentration of LiCl is 16g / L), stir well, after making it fully dissolved, add 0.40 g5, (6) diaminobisbenzimidazole, 7.2ml of acid absorbent pyridine (the concentration of pyridine is 24ml / L), stir until fully dissolved and mixed evenly, then add 9.53g of PPD (PPD and 5, (6) di The total concentration of aminobenzimidazole is 0.3 mol / L, the molar ratio of PPD to 5, (6) diaminobenzimidazole is 98:2), stir until completely dissolved, and then pass through a condensation bath at -5°C, After the connection is completed, add TPC three times, add 6.09g each time (the total concentration of TPC is 0.3mol / L), stir to make it fully react, at this time increase the speed to 3000r / min, when the rod climbing phenomenon occurs, withdraw Drop the condensed oil bath, and continue the reactio...

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Abstract

The invention relates to a polymerization method capable of effectively controlling the phase transformation in a PPTA (poly-p-phenylene terephthamide) synthesis process. The polymerization method comprises the following steps of firstly dissolving LiCl in a solvent NMP (N-methyl-2-pyrrolidone) under the condition of nitrogen atmosphere protection, then adding comonomer p-phenylenediamine, terephthaloyl chloride and trace comonomer, adding acid absorbent pyridine, stirring so as to completely dissolve the acid absorbent pyridine, then adding PPD ((Para Phenylene Diamine), stirring so as to completely dissolve the PPD, then feeding condensing oil bath, maintaining the temperature of the condensing oil bath at -15 DEG C to -5 DEG C, adding TPC (Thymolphthalein Complexone) in three times, and stirring so as to fully react the TPC, thus obtaining modified PPTA resin, wherein the logarithmic viscosity number of the modified PPTA resin is in the range of 5.0-8.0, and the trace comonomer is a diamine monomer containing a flexible chain structure. The polymerization method is a method of effectively increasing the molecular weight by using the phase transformation; and according to the method, the phase transformation time of transforming a liquid phase into a solid phase can be delayed in the polymerization process, so that the molecular weight is effectively increased and the turbidity of a liquid crystal spinning solution is improved.

Description

technical field [0001] The invention relates to a polymerization method for controlling phase transition in the synthesis process of PPTA, in particular to a polymerization method for controlling phase transition in the synthesis process of PPTA which effectively delays the phase transition time. Background technique [0002] Aramid fibers can be roughly divided into poly-m-phenylene isophthalamide fiber (referred to as meta-aramid fiber), poly-para-phenylene terephthalamide fiber (referred to as para-aramid fiber) and heterocyclic aromatic polyamide fiber. Amide fiber (referred to as aramid fiber III) and other varieties. Because aramid fibers have the characteristics of ultra-high modulus, high strength, high temperature resistance, and light weight, they are widely used in aerospace, military clothing, and material reinforcement. However, due to the high rigidity of PPTA molecular chains, strong hydrogen bonds between molecular chains, tight packing and high crystallizat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32D01F6/80
Inventor 余木火李双江孔海娟刘静宋福如钟鸿鹏亢春卯邱大龙沈伟波刘新东杜凌栋叶盛宋志强宋利强宋聚强滕翠青韩克清马禹李新霞薛玉清
Owner DONGHUA UNIV
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