Preparation method of poly (p-phenylene terephthamide) spinning solution

A technology of poly-p-phenylene terephthalamide spinning and poly-p-phenylene terephthalamide, which is applied in the field of spinning dope preparation and can solve the problems of long time for defoaming and difficulty in dissolving PPTA, The increase of chlorine content in fibers and other problems can achieve the effect of reducing dissolution time, reducing dissolution time and controlling degradation

Inactive Publication Date: 2015-10-14
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation of para-aramid spinning stock solution is an important part of large-scale industrialization. Chinese patent CN102268743 provides a preparation technology of para-aramid spinning solution. Formamide p-phenylenediamine resin is mixed and dissolved in a twin-screw extruder to obtain an efficient and uniform solution. The disadvantage is that the introduction of co-solvent perchloric acid increases the chlorine content in the spun fibers, which is far more than that of European counterparts. Aramid fiber chlorine content standard
Chinese patent CN1256474 relates to the manufacture method of poly-p-phenylene terephthalamide fiber, wherein, the preparation of spinning solution is provided, the method is to mix PPTA with sulfuric acid with a concentration greater than 99%, and enter it in a twin-screw extruder Dissolving and defoaming, this method of preparing spinning solution, the water brought in by impure sulfuric acid will make it difficult to dissolve and lead to the degradation of PPTA
This solid-liquid dissolution method itself takes a long time to dissolve, and in the air, stirring will cause the solution to generate a large number of bubbles, and it will take a long time to defoam, which will lead to polymer degradation and also cause polymer degradation.
Solid-liquid two-phase mixing, the solution may also produce inhomogeneity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 8g of poly-p-phenylene terephthalamide powder (inherent logarithmic viscosity is 6.2dL / g) passing through a 140-mesh sieve with a high-precision measuring electronic scale, and place it in a continuous vacuum drying device at a temperature of 120°C Completely dry to a water content of 55ppm, cool and freeze to -15°C; use the same weighing method, weigh 72g of sulfuric acid with a concentration of 100.2%, place the weighed concentrated sulfuric acid in a freezing environment at -15°C, cool and solidify, Then crush it into fine powder, pass through a 200 mesh sieve, put the two kinds of powder into the first-stage twin-screw extruder and mix for 1 hour, and then transport the mixed powder to the second-stage belt under the vacuum condition of residual pressure of 10mmHg Dissolution is carried out in a temperature-controlled twin-screw extruder with a vacuum pump. Dissolution conditions, the temperature rises from -15°C to 40°C and stays for 10 minutes, and finally ri...

Embodiment 2

[0034] Weigh 20g of poly-p-phenylene terephthalamide powder (inherent logarithmic viscosity is 6.2dL / g) through 140 meshes by using high-precision metering electronics, and place it in a vacuum drying device at a temperature of 82°C to dry to a water content of 100ppm , cooled and frozen to 5°C; using the same weighing method, weigh 48g of sulfuric acid with a concentration of 100.2%, place the weighed concentrated sulfuric acid in a solidification device at 5°C to freeze and solidify, and then crush it into fine powder, pass 200 Mesh sieve, put the two powders into the mixing tank for 1.5h of mixing, and then transfer the mixed powder to a temperature-controlled twin-screw extruder with a vacuum pump under a vacuum with a residual pressure of 9mmHg for dissolution , Dissolving conditions, the temperature is gradually raised from 5°C to 20°C, stay for 1 hour, and finally rise to 100°C, the heating rate is 1°C / min, the whole dissolution process dissolves for 155min, forming a un...

Embodiment 3

[0036] Weighed 12.5g of poly-p-phenylene terephthalamide powder (inherent logarithmic viscosity: 6.2dL / g) over 140 meshes with a high-precision metering electronic scale, and placed it in a vacuum drying device at a temperature of 102°C. Dry to water content of 60ppm, cool and freeze to -2°C; use the same weighing method, weigh 57.5g of concentrated sulfuric acid with a concentration of 100.5%, place the weighed concentrated sulfuric acid in a freezing and solidifying device at -2°C, and cool Solidify, then pulverize into fine powder, pass through 200 meshes, put the two powders into the mixing tank for 1 hour and mix thoroughly, and then transport the mixed powder to a vacuum pump with a vacuum pump under a vacuum with a residual pressure of 8mmHg, which can be controlled by temperature. Dissolve in a stirred tank, maintain a vacuum residual pressure of 8mmHg during the dissolution, gradually increase the temperature from -2°C to 30°C, stay for 30 minutes, and finally graduall...

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PUM

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Abstract

The invention relates to a preparation method of a poly (p-phenylene terephthamide) spinning solution. The preparation method comprises the steps that vacuum drying and freezing treatment are conducted on poly (p-phenylene terephthamide), and treated poly (p-phenylene terephthamide) is obtained; concentrated sulfuric acid is cooled, solidified and smashed; the treated poly (p-phenylene terephthamide) and treated concentrated sulfuric acid are mixed at a low temperature to obtain a solid solution, a vacuum condition is created, and the solid solution is heated up and dissolved to form the spinning solution. According to the preparation method of the poly (p-phenylene terephthamide) spinning solution, two powdered substances are fully mixed, the mixing efficiency is high, and the dissolving time is greatly reduced; the vacuum condition is created before the dissolving process is conducted, bubbles are not produced in the solution, the deaeration process is omitted, and degradation of the polymer is greatly slowed down; the whole dissolving process is simple and easy to carry out, and the industrial production of high-quality poly (p-phenylene terephthamide) fibers is facilitated.

Description

technical field [0001] The invention belongs to the field of preparation of spinning stock solution, in particular to a preparation method of poly-p-phenylene terephthalamide. Background technique [0002] Polyparaphenylene terephthalamide fiber is called para-aramid fiber or aramid fiber 1414 (PPTA), which has excellent properties such as high strength, high modulus, resistance to organic solvents, and light weight. The strength is 5-6 times that of high-quality steel. times, the modulus is 2-3 times that of steel and glass fiber, and the density is only 1 / 5 of that of steel. Therefore, the fiber spun has the reputation of "artificial steel wire", and is widely used in national defense, armor and aviation. Aerospace and other special fields. [0003] Due to its broad application background, countries with technology, such as the United States and Japan, strictly block their technology, while non-owner countries are developing production technologies that can be industriali...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01D1/02
Inventor 胡祖明于俊荣陈蕾马禹丁彬胡文兵诸静王彦
Owner DONGHUA UNIV
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