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Method for producing polymetaphenylene isophthamide spinning solution

A technology of polym-phenylene isophthalamide spinning and isophthaloyl chloride, which is applied in the direction of spinning solution preparation, one-component polyamide artificial filament, one-component synthetic polymer rayon, etc. It can solve the problems of large heat transfer area, poor heat transfer effect, and short material residence time, so as to achieve good mass transfer effect and avoid material loss.

Inactive Publication Date: 2010-11-03
四川辉腾科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the disadvantages of poor heat exchange effect, short material residence time and low viscosity of the polymer produced in the preparation of polym-phenylene isophthalamide spinning solution in the prior art, and provide a Preparation method of polym-phenylene isophthalamide spinning solution with large heat exchange area and long material residence time

Method used

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  • Method for producing polymetaphenylene isophthamide spinning solution
  • Method for producing polymetaphenylene isophthamide spinning solution

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Embodiment 1

[0041] The production device used in the production of polym-phenylene isophthalamide in this embodiment includes a precondensation reactor 1, a mixer 2, a self-cleaning tubular reactor 3, a twin-screw kneader 4, and a filter 5. The polycondensation reactor 1 is a tank reactor equipped with a cooling coil, and the self-cleaning tubular reactor 3 is formed by sequentially connecting 4 straight pipes with jackets and 3 bent pipes, and the jackets There is a constant temperature liquid inlet 306 and a constant temperature liquid outlet 307 on the top, and the inside of the jacket is ice salt water. The two ends of the reactor are respectively equipped with a feed port 304 and a discharge port 305. The diameter of each straight pipe of the reactor is 0.15m , the length is 5m, the total length of the straight pipe is 20m, the straight pipe is provided with a stirring shaft 301 connected to the motor, the stirring shaft 301 is provided with a continuous spiral blade 302, the edge of ...

Embodiment 2

[0050] The production device of this embodiment is the same as that of Embodiment 1.

[0051] The method for producing the polym-phenylene isophthalamide spinning solution that the present embodiment enumerates may further comprise the steps:

[0052] (1) Preparation of materials: prepare materials according to the equimolar ratio of m-phenylenediamine (MPD) and isophthaloyl chloride (IPC) (the weight ratio of MPD and IPC is MPD:IPC=1:1.88);

[0053] (2) Precondensation: Dissolve m-phenylenediamine in the organic polar solvent DMAC according to the weight ratio of adding 1 kg of m-phenylenediamine per 8.0 kg of solvent, and add the obtained MPD organic solution to a kettle with a cooling coil Type reactor 1, lower the temperature to about -12°C ~ -10°C, add 1.69kg IPC for every 1kg of m-phenylenediamine, add IPC to the MPD organic solution (the amount of IPC added is 90% of the total amount of IPC) for pre-condensation reaction , the precondensation reaction time is about 45m...

Embodiment 3

[0058] The production device of this embodiment is the same as that of Embodiment 1.

[0059] The method for producing the polym-phenylene isophthalamide spinning solution that the present embodiment enumerates may further comprise the steps:

[0060] (1) Preparation of materials: prepare materials according to the equimolar ratio of m-phenylenediamine (MPD) and isophthaloyl chloride (IPC) (the weight ratio of MPD and IPC is MPD:IPC=1:1.88);

[0061] (2) Precondensation: Dissolve m-phenylenediamine in DMAC, an organic polar solvent, according to the weight ratio of adding 1 kg of m-phenylenediamine per 10.7 kg of solvent, and add the obtained MPD organic solution to a kettle with a cooling coil Type reactor 1, lower the temperature to about -15°C, add 1.59kg IPC to MPD organic solution according to every 1kg m-phenylenediamine, add IPC (the amount of IPC added is 85% of the total amount of IPC) to carry out pre-condensation reaction, pre-condensation reaction The time is abou...

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Abstract

The invention relates to a tube-type continuous method for producing polymetaphenylene isophthamide spinning solution, which is characterized in that a method for serially connecting a self-cleaning tubular reactor serving as a condensation reactor and a twin-screw kneading machine serving as a neutralization reactor is adopted for preparing the polymetaphenylene isophthamide spinning solution. The self-cleaning tubular reactor solves the problems that side reactions are increased due to quick generation of heat in the reaction and the polymer molecular weight cannot be improved; and the twin-screw kneading machine solves the problem of poor dissolution of solid granules in the spinning solution caused by nonuniform liquid / solid kneading in the neutralization process. The preparation method comprises the steps of pre-condensation, condensation, neutralization, and forced extrusion and filtration. The solid content of the final spinning solution is 14 to 20 percent; and calcium hydroxide is adopted for neutralization by one step, and the calcium chloride content is 6.5 to 9.3 percent. If the calcium hydroxide and sodium hydroxide are adopted for neutralization by two steps, the calcium chloride content can be less than 3 percent. Therefore, the method is also suitable for producing spinning solution for a high salt method and a low salt method.

Description

technical field [0001] The invention relates to a method for continuously producing polym-phenylene isophthalamide spinning solution, which belongs to the technical field of fiber synthesis. Background technique [0002] Poly(m-phenylene isophthalamide) is a material with flame retardant, high temperature resistance, corrosion resistance and excellent electrical insulation properties. It is used in the production of high temperature fireproof clothing, high temperature resistant filter materials, high temperature resistant insulating paper and as a It has been widely used in the production of wear-resistant materials and fillers. [0003] At present, the methods for producing poly-m-phenylene isophthalamide mainly include interfacial polycondensation method and low-temperature solution polycondensation method, each of which has many patents and literature reports. The interfacial polycondensation method is to dissolve isophthaloyl chloride in an organic solvent immiscible w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/60D01D1/02C08G69/32
CPCD01D1/02D01F6/605
Inventor 张胜才潘育英韩和平石和平张鸥
Owner 四川辉腾科技股份有限公司
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