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A kind of preparation method of meta-aramid fiber spinning glue

A glue and liquid technology, applied in the field of aramid fiber production, can solve the problems of reduced product performance, more waste, and increased difficulty in controlling polymerization viscosity, and achieve the effect of low cost and high quality

Inactive Publication Date: 2016-01-20
SICHUAN PROVINCE JINLU RESIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In the disclosed production technology of m-aramid spinning glue, most of them use m-phenylenediamine (MPD) to add polar solvent, control the temperature of the reaction system at -10-10°C, and gradually add isophthaloyl dichloride (IPC) reaction until the reaction is completed, then adjust the pH value of the reaction solution to neutral, and then filter to obtain the spinning stock solution. It is difficult to stabilize the product quality by using such a one-step reaction method, and excessive addition of isophthaloyl chloride often occurs , resulting in more waste in a single batch; the hydrochloric acid produced in the polymerization process, the prior art is to use hydroxide as a neutralizing agent to neutralize, and the reaction of hydrochloric acid and hydroxide will generate a large amount of water in the neutralization process, and the generated water It will also lead to the decomposition of isophthaloyl dichloride. It should be pointed out that isophthaloyl dichloride and m-phenylenediamine have high chemical activity and are easily invalidated by external influences. Due to the presence of water after neutralization, the The polymerization reaction cannot be carried out completely, and it may also cause the reaction solution to become dark and form cross-linking of the polymer, which makes the spinnability of the polymer solution worse and the performance of the product decreases
[0003] At the same time, in the process of using hydroxide to neutralize the hydrochloric acid produced by the polymerization reaction, a large amount of hydroxide precipitates, such as calcium hydroxide or magnesium hydroxide, will also be produced. The large amount of precipitates will make it difficult to control the polymerization viscosity, and form The diameter of the precipitated hydroxide atoms is large, and the traditional technical approach is used to filter once after the neutralization is completed. A large amount of precipitation makes the filtration of the polymer solution more difficult, and the service life and operation cycle of the filtration equipment are significantly shortened. On the one hand, it is not conducive to Production, on the other hand, in the process of frequent replacement of filter media and cleaning of filter equipment, a large amount of loss of polymer solution will be caused
[0004] The above unfavorable factors will cause a substantial increase in production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Carry out prepolymerization reaction in the first polymerization still, m-phenylenediamine is dissolved in monomethyl acetamide, and its concentration is 4%, and the liquid isophthaloyl chloride (isophthaloyl dichloride (isophthaloyl dichloride) of dehydration treatment is slowly added therein simultaneously Formyl chloride is heated and melted with jacketed water), and continues to be added until the reaction forms an oligomer solution with a degree of polymerization of 85%. The medium dynamic viscosity is maintained within 1500 centipoise, and then the pH value of the reaction solution is adjusted to 3.5 by adding ammonia gas, and then the first filter is carried out, and the obtained oligomer solution is transferred to the second polymerization tank for post-polymerization reaction; to the second polymerization tank Add isophthaloyl chloride until the reaction is complete to obtain polymer glue. The reaction temperature is controlled at 35-45°C. During the reaction, t...

Embodiment 2

[0028] The process and parameters of this example are basically the same as those of Example 1, except that the neutralizing agent I used in this example is ethylenediamine, and the neutralizing agent II is N,N-dimethylbutyramide.

Embodiment 3

[0030]Carry out prepolymerization reaction in the first polymerization tank, dissolving m-phenylenediamine in dimethylacetamide, its concentration is 10%, slowly adds the liquid isophthaloyl chloride (isophthaloyl dichloride (isophthaloyl dichloride) of dehydration treatment wherein Formyl chloride is heated and melted with jacketed water), continue to add until the reaction forms an oligomer solution with a degree of polymerization of 90% The dynamic viscosity remains within 1500 centipoise, then add methylamine to adjust the pH value of the reaction solution to 4.5 and carry out the first filter, and the gained oligomer solution is transferred to the second polymerizer for post-polymerization; Add isophthaloyl dichloride until the reaction is complete to obtain polymer glue. The reaction temperature is controlled at 35-45°C. During the reaction process, the dynamic viscosity is maintained at 40,000-50,000 centipoise. After the polymerization reaction is complete, add ethylene...

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Abstract

The invention discloses a preparation method of meta-aramid spinning glue, which belongs to the technical field of aramid fiber production; the preparation method of meta-aramid spinning glue adopts the principle of intermittent low-temperature polycondensation, and the preparation process Pioneering two-step polymerization, two-step neutralization segmented multi-channel filtration process, and the introduction of new organic solvents and neutralizers, by controlling the reaction temperature and adjusting the pH value, it overcomes the neutralization process of the existing process Unfavorable factors such as water affecting product quality, difficulty in controlling polymerization viscosity, and large loss of equipment and raw materials caused by difficult filtration will ultimately result in a product solution with higher quality and lower cost.

Description

technical field [0001] The invention relates to an organic polymerization process method, in particular to a method for preparing meta-aramid fiber spinning glue, and belongs to the technical field of aramid fiber production. Background technique [0002] In the disclosed production technology of m-aramid spinning glue, most of them use m-phenylenediamine (MPD) to add polar solvent, control the temperature of the reaction system at -10-10°C, and gradually add isophthaloyl dichloride (IPC) reaction until the reaction is completed, then adjust the pH value of the reaction solution to neutral, and then filter to obtain the spinning stock solution. It is difficult to stabilize the product quality by using such a one-step reaction method, and excessive addition of isophthaloyl chloride often occurs , resulting in more waste in a single batch; the hydrochloric acid produced in the polymerization process, the prior art is to use hydroxide as a neutralizing agent to neutralize, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/46C08G69/32D01F6/60
Inventor 张培林杜庆丰冯将军
Owner SICHUAN PROVINCE JINLU RESIN