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Semi-continuous preparation method for solution of heterocycle-containing aromatic polyamide copolymer

A semi-continuous technology for aromatic polyamides, which is applied in the field of semi-continuous preparation of heterocyclic-containing copolymerized aromatic polyamide solutions, which can solve the problems of low molecular weight of polymerization products, uneven solution, difficult mass transfer and heat transfer of the system, etc. , to achieve the effect of improving uniformity, increasing molecular weight and reducing side reactions

Inactive Publication Date: 2011-03-16
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, with the further progress of the reaction, the shortcomings of this method are fully exposed. As the dynamic viscosity of the system rises sharply, the mass transfer and heat transfer of the system become difficult, which affects the effective collision of the active end groups of the polymer molecular chains. , resulting in lower molecular weight of the polymerized product and uneven solution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a kettle reactor, 4.76 parts of lithium chloride were dissolved in 158 parts of freshly distilled dry DMAc to prepare a mixed solvent, and 1 part of refined PPDA and 3.1 parts of M3 were dissolved in it at -10°C, Then add 4.7 parts of refined TPC for pre-polycondensation, keep the temperature of the system below 10°C, after 30 minutes of reaction, a low-molecular-weight prepolymer is formed. Screw extruder. The temperature of the twin-screw extruder was controlled at 80° C., and a light yellow transparent polymer solution was extruded for about 18 minutes. The inherent viscosity of the polymer was determined to be 6.5 dL / g, and the solution concentration was 4.1%.

Embodiment 2

[0030] In a kettle reactor, 4.2 parts of lithium chloride were dissolved in 141 parts of freshly distilled dry DMAc to prepare a mixed solvent, and 1 part of refined PPDA and 2.54 parts of M3 were dissolved in it at -10°C, Then add 4.18 parts of refined TPC for pre-polycondensation, keep the temperature of the system below 10°C, and react for 30 minutes to generate a low-molecular-weight prepolymer. Screw extruder. The temperature of the twin-screw extruder was controlled at 80° C., and a light yellow transparent polymer solution was extruded for about 18 minutes. The inherent viscosity of the polymer was determined to be 6.3 dL / g, and the solution concentration was 4%.

Embodiment 3

[0032] In a kettle reactor, 3.8 parts of lithium chloride were dissolved in 127 parts of freshly distilled dry DMAc to prepare a mixed solvent, and 1 part of refined PPDA and 2.1 parts of M3 were dissolved in it at -10°C, Then add 3.76 parts of refined TPC for pre-polycondensation, keep the temperature of the system lower than 10 ° C, and react for 30 minutes to generate a low molecular weight prepolymer, which enters a double-stranded polymer with a diameter of 25 mm, an aspect ratio of 1:40, and a rotating speed of 50 rpm. Screw extruder. The temperature of the twin-screw extruder was controlled at 80° C., and a light yellow transparent polymer solution was extruded for about 18 minutes. The inherent viscosity of the polymer was determined to be 6.2 dL / g, and the solution concentration was 4%.

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Abstract

The invention relates to a semi-continuous preparation method for solution of heterocycle-containing aromatic polyamide copolymer, which comprises the following steps of: dissolving p-phenylenediamine and 5(6)-amino-2-(4-aminophenyl)benzimidazole in a mixed solvent system and cooling to -20 to 10 DEG C; adding terephthaloyl chloride (TPC) with stirring to obtain prepolymer; and adding the prepolymer into a double-screw extruder and retaining in the double-screw extruder at the temperature of between 40 and 100 DEG C for 10 to 25 minutes to obtain the solution of heterocycle-containing aromatic polyamide copolymer. The double-screw extruder is taken as a main reactor, so that a reaction interface can be updated, the heat transfer problem of the system can be solved, the low-temperature solution polycondensation of the heterocycle-containing aromatic polyamide copolymer is semi-continuous, the side reaction is reduced, and the molecular weight of the polymer is effectively improved.

Description

technical field [0001] The invention belongs to the field of preparation of a heterocyclic ring-containing copolymerized aromatic polyamide solution, in particular to a method for semi-continuously preparing a heterocyclic ring-containing copolymerized aromatic polyamide solution. Background technique [0002] Heterocycle-containing copolymerized aromatic polyamide fiber (heterocyclic aramid fiber for short) is a kind of polymer fiber whose main chain is composed of aromatic ring and heterocyclic ring. It has the characteristics of high strength, high modulus and high temperature resistance. The main material of rocket engine casing, body armor, and tank composite armor has an irreplaceable position with other high-strength and high-modulus fibers in some application fields of the defense industry. [0003] One of the keys to the preparation of high-performance heterocyclic aramid fibers is to obtain a uniform polymer solution with high molecular weight and narrow molecular ...

Claims

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Application Information

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IPC IPC(8): C08G69/32C08G69/28B29C47/92B29C48/92
CPCB29C48/92B29C2948/9259B29C2948/92704B29C2948/92885B29C2948/92895
Inventor 陈蕾胡祖明于俊荣诸静高宝山
Owner DONGHUA UNIV
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