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Industrial method for preparing PPTA spinning slurry with solid sulphuric acid

A technology of solid sulfuric acid and slurry, which is used in spinning solution preparation, filament forming treatment, textile and papermaking, etc., can solve the problems that extrusion conditions affect the uniformity of liquid crystal solution, solid sulfuric acid needs to be prepared separately and is difficult to obtain, etc. Excellent self-cleaning effect, excellent mixing effect, and the effect of reducing resin degradation

Active Publication Date: 2009-10-14
中国平煤神马控股集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But it has the following problems when it is used: (1) solid sulfuric acid needs to be prepared separately; (2) due to the use of single-shaft stirred tank mixing in the patent, heating, kneading and extrusion in the single-screw extruder, due to sandy The content of sulfuric acid in the product is not the same, and it is difficult to obtain uniform PPTA / H when it is heated and dissolved in a single-screw extruder 2 SO 4 liquid crystal slurry
In addition, in the process of continuously preparing the liquid crystal solution, the fluctuations in metering and extrusion conditions will affect the uniformity of the liquid crystal solution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 180 kilograms of solid sulfuric acid with a concentration of 100.1% and 45 kilograms of dry PPTA resin with a logarithmic reduced viscosity of 6.0 are added to a three-axis planetary mixer with an effective volume of 300 liters. The stirring speed is 120 rpm and the jacket temperature is 0 Mix at -3°C for 20 minutes, then pass hot water at 95°C into the jacket, heat up to the mixture is completely dissolved while stirring and vacuuming, the temperature of the melt is controlled at 75°C, and the total residence time is about 2 hours. Then use the screw pump at the bottom of the tank to add the slurry to a continuous biaxial mixer and kneader at a speed of 1.25 kg / min for mixing, kneading, and shearing to form a uniform liquid crystal slurry. The screw diameter of the twin-shaft mixing and kneading machine is 75mm, L / D=40, mixing, kneading and extruding into a mixing batch with a volume of 300 liters, defoaming In the kettle, the temperature is 80°C and the pressure is 0...

Embodiment 2

[0021]Add 180 kg of liquid sulfuric acid with a concentration of 100.1% into a three-axis planetary mixer with an effective volume of 300 liters, stir for 30 minutes at a stirring speed of 120 rpm and a jacket temperature of -10 to 0 ° C, and let the liquid sulfuric acid form a solid Sulfuric acid, then add 45 kg of dry PPTA resin with a logarithmic reduced viscosity of 6.0 and mix for 20 minutes; then pass hot water at 100°C into the jacket, and heat up to the mixture completely dissolved while stirring and vacuumizing. The temperature of the melt is controlled at 85° C., and the residence time of PPTA / H2SO4 is about 2 hours, and then the slurry is added to the continuous twin-shaft mixing and kneader with a screw pump at a speed of 1.25 kg / min. The screw diameter of the twin-shaft mixing and kneading machine is 75mm, L / D=40, and the jacket temperature is 85°C, and the rotation speed is 120rpm. Mixing, kneading and extruding into a mixing batch with a volume of 300 liters, def...

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Abstract

The invention discloses an industrial method for preparing PPTA spinning slurry with solid sulphuric acid, comprising the following steps: (1) granular solid sulphuric acid and dried PPTA resin with logarithmic viscosity number of 4.0-8.0dl / g are fully mixed, and are prepared into a liquid crystalline solution containing 16-23 percent of PPTA by weight percent via heating dissolving and pre-deaeration; (2) the obtained liquid crystalline solution is mixed, kneaded and sheared to form uniform liquid crystalline slurry under the temperature of 60-100 DEG C; and (3) the formed liquid crystalline slurry is further mixed and deaearted under the conditions of the temperature of 60-100 DEG C and the pressure of 0.09MPa to obtain stable and uniform PPTA / H2SO4 liquid crystalline solution, i.e. spinning solution. The method has good mixing effect, can rapid extrude under high shearing rate without the degradation of the liquid crystalline solution caused by high shearing rate and high temperature.

Description

technical field [0001] The invention relates to an industrialized method for preparing poly-p-phenylene terephthalamide (PPTA) spinning slurry, in particular to an industrialized method for preparing PPTA spinning slurry with solid sulfuric acid. Background technique [0002] PPTA fiber is a high-performance fiber. Due to its excellent physical and mechanical properties such as high strength, high modulus, high temperature resistance, and corrosion resistance, it has been widely used in national defense, aerospace, aviation, transportation and other fields. As early as the early 1970s, DuPont of the United States invented the technology of manufacturing PPTA fibers by dry jet-wet spinning, and one of the key technology is PPTA / H 2 SO 4 Liquid crystal solution, that is, the preparation of spinning slurry, because the powdery PPTA resin heats up rapidly when dissolved in sulfuric acid solution, it is very easy to dissolve and agglomerate on the surface, making it difficult fo...

Claims

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Application Information

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IPC IPC(8): D01D1/02D01D1/10D01F6/60
Inventor 李磊潘育英吕清海马源王良郑淑昀王建民罗亚利张会云梁海军
Owner 中国平煤神马控股集团有限公司
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