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A kind of method that ppta resin directly prepares aramid fiber spinning slurry

A resin, direct technology, applied in the direction of spinning solution preparation, single-component polyamide artificial filament, etc., can solve the problems of unfavorable production efficiency, long time consumption, large resin degradation, etc., to shorten the preparation time and improve the dissolution efficiency High, accelerated dissolution effect

Active Publication Date: 2016-08-17
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the resin powder particles are small and the specific gravity is smaller than that of sulfuric acid particles, the form of the mixture formed is that many resin particles are adsorbed on the surface of the sulfuric acid particles, which is equivalent to the uniform dispersion of sulfuric acid in the resin, and a certain degree of agglomeration will still occur.
In addition, concentrated sulfuric acid needs to be frozen, which takes a long time, causes large resin degradation, and consumes a lot of energy, which is not conducive to improving production efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 100 kg of PPTA resin with an inherent viscosity of 6.0dl / g and a water-to-resin mass ratio of 1:1.2 after washing with water into a multi-axis planetary mixer for stirring. Pass through the freezing liquid to control the temperature of the wet resin at about 1°C.

[0021] Slowly inject 5MPa of SO into the wet resin 3 gas, keeping the system temperature at 11°C. After 0.8h, the water in the resin absorbs SO 3 concentration reaches 80%, the SO 3 The amount of gas increased, and after 10 minutes, the concentration of sulfuric acid reached 99.8%.

[0022] The temperature of the mixture was raised to 85° C. for dissolution and pre-defoaming, and a 18.1% PPTA / sulfuric acid liquid crystal solution was obtained after 0.5 h.

Embodiment 2

[0024] Add 100 kg of PPTA resin with an inherent viscosity of 5.8dl / g and a water-to-resin mass ratio of 1:1.6 after washing with water into a multi-axis planetary agitator for stirring. Pass through the freezing liquid to control the temperature of the wet resin at about 1°C.

[0025] Slowly inject 5MPa of SO into the wet resin 3 gas, keeping the system temperature at 11°C. After 0.6h, the water in the resin absorbs SO 3 concentration reaches 80%, the SO 3 The amount of gas increased, and after 10 minutes, the concentration of sulfuric acid reached 99.9%.

[0026] The mixture is heated to 85°C for dissolving and pre-defoaming. After 0.4h, a liquid crystal solution of PPTA / sulfuric acid is obtained. The obtained liquid crystal solution is pumped into the subsequent channel for defoaming, and a uniform concentration of 22.7% is obtained as PPTA / sulfuric acid. Spinning slurry.

Embodiment 3

[0028] Add 100 kg of PPTA resin with an inherent viscosity of 7.8dl / g and a water-to-resin mass ratio of 1:1.1 that has been washed with water into a multi-axis planetary mixer for stirring. Pass through the freezing liquid to control the temperature of the wet resin at about 1°C.

[0029] Slowly inject 10MPa of SO into the wet resin 3 gas, keeping the system temperature at 13°C. After 0.5h, the water in the resin absorbs SO 3 concentration reaches 80%, the SO 3 The amount of gas increased, and after 10 minutes, the concentration of sulfuric acid reached 100.1%.

[0030] The mixture was heated to 85°C for dissolving and pre-defoaming. After 0.5h, a liquid crystal solution of PPTA / sulfuric acid was obtained. The obtained liquid crystal solution was pumped into the subsequent channel for defoaming, and a uniform and stable concentration of 16.8% PPTA / sulfuric acid was obtained. silk slurry.

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PUM

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Abstract

The invention relates to a method for directly preparing an aramid spinning solution from PPTA (p-phenylene terephthalamide) resin. The method comprises the steps of directly washing the synthesized PPTA resin with water after neutralization, dehydrating the PPTA resin to form dehydrated PPTA resin, cooling the dehydrated PPTA resin, supplying SO3 gas under a mixing condition, keeping the temperature of a system at 11-13 DEG C to form concentrated sulfuric acid, heating to 80-90 DEG C for dissolution and pre-defoamation to form a liquid crystal solution, and defoaming the liquid crystal solution. The method has good mixing effect and high dissolution efficiency, and greatly shortens the preparation time from the resin to the spinning solution, and less resin is degraded during the dissolution.

Description

technical field [0001] The invention belongs to the field of preparation of spinning slurry, in particular to a method for directly preparing aramid spinning slurry with PPTA resin. Background technique [0002] Poly(p-phenylene terephthalamide) (PPTA) fiber is a high-performance fiber widely used in various fields. It is prepared from liquid crystal solution of PPTA resin / concentrated sulfuric acid by dry jet wet spinning. At present, the industrial preparation method of PPTA resin / concentrated sulfuric acid spinning slurry is mainly to directly mix fully dried resin with concentrated sulfuric acid, shear, and heat up to dissolve. There are also patent reports that PPTA resin is first mixed with frozen concentrated sulfuric acid, and then heated and sheared to form a liquid crystal slurry. For the traditional spinning slurry preparation method, the surface of the resin swells rapidly after being in contact with it, heats up and sticks to each other, resulting in serious a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/90D01F1/10D01D1/02D01D1/10
Inventor 胡祖明刘兆峰马禹丁彬胡文兵陈蕾王彦诸静于俊荣
Owner DONGHUA UNIV