Device and method for efficiently dissolving poly(p-phenytene terephthalamide) resin

A technology of p-phenylene terephthalamide and poly-p-phenylene terephthalamide is applied in the field of spinning solution preparation of poly-p-phenylene terephthalamide, and can solve the problems of uneven dissolution, limited dehydration capacity, uneven distribution of sulfuric acid and the like , to achieve the effect of improving the dissolution effect, reducing the gel particles and reducing the agglomeration phenomenon

Active Publication Date: 2013-04-03
上海舟汉纤维材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the 1970s, my country began to develop poly-p-phenylene terephthalamide fibers, and made great progress, but there are still technical problems that high-viscosity poly-p-phenylene terephthalamide is difficult to dissolve and defoam. , the reason is that the poly-p-phenylene terephthalamide / H2S04 solution system has a high viscosity and uneven stirring and mixing, resulting in uneven dissolution and incomplete defoaming. Furthermore, the solution system cannot stay for a long time, otherwise it will be easy Leading to the degradation of poly-p-phenylene terephthalamide during the dissolution process, it is impossible to meet the requirements of stable and continuous production. Many factors have led to the delay in the industrialization of poly-p-phenylene terephthalamide fiber in my country. one of the factors
[0004] Chinese patent CN101555631A discloses a method for dissolving poly-p-phenylene terephthalamide with solid sulfuric acid. The method uses 98-100.3% concentrated sulfuric acid at a temperature of -15°C to -5°C to make granular solids Sulfuric acid, and then mix it with poly-p-phenylene terephthalamide resin and dissolve it. The advantage of this method is that it solves the problem of metering concentrated and convenient sulfuric acid. High, the sulfuric acid in the system is unevenly distributed in the slurry, resulting in uneven dissolution and easy generation of gel particles, which still cannot solve the problem of uniform dissolution
[0005] Chinese patent CN1693543A discloses a method for continuously preparing poly-p-phenylene terephthalamide fibers. The method uses 98-100% concentrated sulfuric acid and poly-p-phenylene terephthalamide at a temperature of 50°C to 100°C. P-phenylenediamine resin is continuously added to two twin-screw extruders for dissolution. This method achieves the goal of continuous preparation, but the temperature is relatively high, and it is easy to dissolve in the mixture of concentrated sulfuric acid and poly-p-phenylene terephthalamide resin. Agglomeration occurs during the process, resulting in insufficient local dissolution and a "white core" phenomenon. At the same time, due to the limited dehydration ability of the 98-100% concentrated sulfuric acid used, it is impossible to completely remove the interpolymers in poly-p-phenylene terephthalamide. Moisture, so there is still degradation during dissolution

Method used

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  • Device and method for efficiently dissolving poly(p-phenytene terephthalamide) resin
  • Device and method for efficiently dissolving poly(p-phenytene terephthalamide) resin

Examples

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Effect test

example 1

[0030] Using a liquid mass flowmeter and a high-precision loss-in-weight continuous metering electronic scale, the mixed acid of 99.4% concentrated sulfuric acid and 5% phosphorus pentoxide and polyterephthalamide with a logarithmic viscosity of 6.5dl / g The diamine resin is added with the feed rate of 60.00g / min and 15.00g / min and the diameter is φ125mm, the ratio of length to diameter is 8:1, co-rotating, the temperature of the twin-screw extruder that the rotating speed is 330rpm is 15 ℃, and the residence time is 30min, fully mixed, the extruded material is fed into the introduction area of ​​a twin-screw extruder with a diameter of φ300mm, an aspect ratio of 10:1, co-rotating, and a speed of 70rpm. The temperature is 85°C and the residence time is 20min. The degassing zone of the two extruders is externally connected with vacuum pumping, the vacuum degree is 4KPa, and the pressure in the pressurized zone is 5MPa, and the dissolved slurry is degassed.

[0031] After being m...

example 2

[0033] Using a liquid mass flowmeter and a high-precision loss-in-weight continuous metering electronic scale, the mixed acid of 99.4% concentrated sulfuric acid and 5% perchloric acid and the logarithmic viscosity of 5.6dl / g poly terephthalamide The amine resin is fed into a twin-screw extruder with a diameter of φ125mm, an aspect ratio of 8:1, and a rotation speed of 330rpm at a feeding rate of 60.00g / min and 15.00g / min. The temperature is 15°C and the residence time is 30min. , fully mixed, the extruded material is fed into the introduction area of ​​a twin-screw extruder with a diameter of φ300mm, an aspect ratio of 10:1, co-rotating, and a rotating speed of 70rpm. The temperature is 85°C and the residence time is 20min. The degassing zone of the two extruders is externally connected with vacuum pumping, the vacuum degree is 4KPa, and the pressure in the pressurized zone is 5MPa, and the dissolved slurry is degassed.

[0034]After being metered and filtered, the extruded s...

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Abstract

The invention discloses a device and a method for efficiently dissolving poly(p-phenytene terephthalamide) resin, belongs to the field of polymer material manufacture, and relates to a high-polymer fiber material processing technology, in particular to a technology for preparing a poly(p-phenytene terephthalamide) spinning solution. The key points are that: a preparation device is used and the method comprises the following steps of: preparing a solvent for dissolving poly(p-phenytene terephthalamide); adding the solvent and dried poly(p-phenytene terephthalamide) resin with logarithmic specific concentration viscosity of 4.0-8.5dl / g into a first twin-screen extruder; and tightening a second twin-screw extruder to obtain high-efficiency uniformly dissolved slurry. The invention has the advantages that: defects in the prior art are overcome, and a process and a device suitable for industrial continuous high-efficiency and high-quality production are realized.

Description

technical field [0001] The invention belongs to the field of polymer material manufacturing and relates to the processing technology of polymer fiber materials, specifically the technology of preparing poly(p-phenylene terephthalamide) spinning solution. Background technique [0002] Poly-p-phenylene terephthalamide fiber, commonly known as para-aramid fiber in my country, belongs to aromatic polyamide fiber. It is a fiber with high strength, high modulus, low specific gravity, chemical solvent resistance, high temperature resistance and flame retardancy High-performance materials are widely used in aerospace, military industry, electromechanical, construction, automobile, sporting goods and other fields. [0003] In the 1970s, my country began to develop poly-p-phenylene terephthalamide fibers, and made great progress, but there are still technical problems that high-viscosity poly-p-phenylene terephthalamide is difficult to dissolve and defoam. , the reason is that the poly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01D1/02
Inventor 金伟周文奎刘岳新
Owner 上海舟汉纤维材料科技股份有限公司
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