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A method for preparing aromatic polyamide fiber by adopting a micro-reactor

A technology of microreactor and polymerization reactor, which is applied in the direction of single-component polyamide rayon, fiber chemical characteristics, textiles and papermaking, etc., and can solve problems such as unfavorable recycling, unstable product quality, and hazards

Active Publication Date: 2017-09-26
FININGS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The low-temperature solution polycondensation method using DMF, NMP, etc. as solvents is the main synthesis method of commercial aramid fiber, but this method also has certain problems: (1) The product quality is unstable, because DMF, NMP, etc. are substances that are easy to absorb water, And this reaction system requirement is moisture content below 200ppm, and the existence of moisture has fatal harm to this reaction, causes the sharp reduction of molecular weight, and the dehydration of DMF, NMP and the control of moisture in the reaction system have certain difficulty; (2) Solvent recovery is difficult, and production sewage is difficult to handle. After the reaction, the solvent DMF or NMP must be washed away with water. Since DMF or NMP is very soluble in water and difficult to separate, it is difficult to recover the solvent. In addition, organic substances such as pyridine added to the reaction system Alkaline acid absorbent, which is also unfavorable for the recovery of solvents such as DMF and NMP

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The method for preparing aramid fibers using a microreactor comprises the following steps:

[0054] 1) In a pressure batching kettle equipped with an agitator and connected with a dry nitrogen pipe, add 4.80 g of p-phenylenediamine, add 1.8 g of acid-binding agent triethylamine, replace the original gas with nitrogen, and inject 33.6 g of liquid carbon dioxide, Keep the temperature in the reactor at 25°C and the pressure at 7MPa. After the substances in the pressure batching tank are dissolved, a mixed solution of p-phenylenediamine-triethylamine-liquid carbon dioxide is produced;

[0055] Ⅱ) In another pressure batching kettle equipped with a stirrer and connected with a dry nitrogen pipe, add 9.02g of terephthaloyl chloride, replace the original gas with nitrogen, inject 90.22g of liquid carbon dioxide, and keep the temperature in the reactor at 25 ℃, the pressure is 7MPa, and the liquid carbon dioxide solution of terephthaloyl chloride is made after the material in t...

Embodiment 2

[0062] The method for preparing aramid fibers using a microreactor comprises the following steps:

[0063] 1) In a pressure batching kettle equipped with an agitator and connected with a dry nitrogen pipe, add 4.80 g of p-phenylenediamine, add 3.14 g of acid-binding agent triethylamine, replace the original gas with nitrogen, inject 72 g of liquid carbon dioxide, and keep The temperature in the reactor is -15°C and the pressure is 3MPa. After the substances in the pressure batching tank are dissolved, a mixed solution of p-phenylenediamine-triethylamine-liquid carbon dioxide is produced;

[0064] Ⅱ) In another pressure batching kettle equipped with a stirrer and connected with a dry nitrogen pipe, add 9.02g of terephthaloyl chloride, replace the original gas with nitrogen, inject 135.3g of liquid carbon dioxide, and keep the temperature in the reactor as - 15°C, the pressure is 3MPa, and the liquid carbon dioxide solution of terephthaloyl chloride is made after the substances ...

Embodiment 3

[0071] The method for preparing aramid fibers using a microreactor comprises the following steps:

[0072]1) In a pressure batching kettle equipped with a stirrer and connected with a dry nitrogen pipe, add 240g of m-phenylenediamine, 179.5g of acid-binding agent triethylamine, and 0.96g of calcium chloride, and replace the original gas with nitrogen , inject 4800g of liquid carbon dioxide, keep the temperature in the reactor at -20°C, and the pressure at 2MPa. After the substances in the pressure batching kettle are dissolved, a mixed solution of m-phenylenediamine-triethylamine-calcium chloride-liquid carbon dioxide is prepared ;

[0073] Ⅱ) In another pressure batching kettle equipped with a stirrer and connected with a dry nitrogen pipe, add 451g of isophthaloyl chloride, replace the original gas with nitrogen, inject 9022g of liquid carbon dioxide, and keep the temperature in the reactor at -20°C , the pressure is 2MPa, and the liquid carbon dioxide solution of isophthal...

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Abstract

The invention relates to a method for preparing aromatic polyamide fiber by adopting a micro-reactor. Liquid carbon dioxide and / or supercritical carbon dioxide are adopted as a solvent. The micro-reactor is adopted as a reactor in a pre-polymerization stage. The polymer intrinsic viscosity and the yield of the aromatic polyamide fiber prepared by the method are high. The solvent recovery rate is high.

Description

technical field [0001] The application relates to a method for preparing aramid fiber, in particular, the application relates to a method for preparing aramid fiber using a microreactor. Background technique [0002] Aramid 1313, 1414 is a kind of polyamide fiber, which is made of polycondensation of (meta-, p-) phthaloyl chloride and (meta-, p-) phenylenediamine and then spun through solution. It is mainly used for anti-atomic radiation, high-altitude and high-speed flight In terms of materials, it can also be used for tire window lines, high temperature resistant clothing materials, honeycomb parts, high temperature line pipes, aircraft fuel tanks, firewalls, reverse osmosis membranes or hollow fibers, etc. for special requirements. The synthesis methods of aramid fibers at home and abroad mainly include: low-temperature solution polycondensation method, direct polycondensation method, ionic liquid polycondensation method, and fuming sulfuric acid polycondensation method. ...

Claims

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Application Information

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IPC IPC(8): C08G69/32C08G69/28D01F6/60
CPCC08G69/28C08G69/32D01F6/605Y02P20/54
Inventor 王农跃闻国强赵全忠邵建明
Owner FININGS CO LTD
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