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Method of preparing polyparaphenyl bracing benzdioxazole fibre

A technology of poly-p-phenylene and benzobisoxazole, which is applied in the field of preparation of poly-p-phenylene benzobisoxazole fiber, can solve the problems of long reaction time, high recycling cost, high equipment requirements, etc. The Effect of Concentrated Logarithmic Viscosity

Active Publication Date: 2006-11-22
DONGHUA UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation of PBO fiber basically adopts 4,6-diaminoresorcinol hydrochloride (DAR hydrochloride) to remove hydrogen chloride, and then carry out polycondensation reaction with terephthalic acid in polyphosphoric acid solvent system to prepare PBO slurries are then carried out by dry-jet wet spinning, and U.S. Patent Nos. 5,534,205 and 5,296,185 (The DowChemical Company) report the manufacture method of PBO fibers, but this method needs to remove HCl gas for a long time for monomer DAR hydrochloride , high equipment requirements, long reaction time; use NH 3 And KOH as lye to neutralize the phosphoric acid in the PBO tow coming out of the coagulation solution, the obtained washing liquid contains P, N and K, because the price of phosphoric acid itself is relatively cheap, the recovery cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] With reference to accompanying drawing 1, 4,6-diaminoresorcinol-terephthalate, polyphosphoric acid and P 2 o 5 According to the weight ratio of 1: 1.5: 0.7 into the pre-condensation reactor, stirred at 80 ° C for 2 hours, then heated to 150 ° C within 3 hours and reacted for 5 hours, and then heated to 180 ° C for 2 hours to obtain The PBO slurry enters the twin-screw reaction extruder with 25mm, length-to-diameter ratio of 40, rotating speed of 15 rpm, and temperature of 180°C. The temperature of the spinneret is 170°C, the specification of the spinneret is 0.2×60 holes, and it passes through a tunnel with a length of 1.5 meters and a temperature of 70°C. The atmosphere in the tunnel contains H 3 PO 4 0.08g / L, side blowing speed 0.1 m / s, spinning speed 150 m / min, nozzle stretching 15 times, the obtained PBO fiber tow immediately enters the coagulation bath containing 5% phosphoric acid and the temperature is 40 ℃, After leaving the coagulation bath, the tow is di...

Embodiment 2

[0021] 4,6-diaminoresorcinol-terephthalate, polyphosphoric acid and P 2 o 5 According to the weight ratio of 1:4:2, put it into the pre-condensation reactor, stir at 90°C for 2 hours, then raise the temperature to 160°C within 3 hours and react for 5 hours, then raise the temperature to 180°C for 2 hours, and the obtained PBO slurry enters 50mm, length-to-diameter ratio of 50, rotating speed of 150 rpm, temperature of 180°C twin-screw reaction extruder continues to react, after being filtered, it enters the metering pump and is sent to the spinneret, and the spinning temperature is 180°C , the size of the spinneret is 0.2×60 holes, passing through a tunnel with a length of 3.0 meters and a temperature of 75°C, the atmosphere in the tunnel contains H 3 PO 4 0.1g / L, side blowing speed 0.3 m / s, spinning speed 150 m / min, nozzle stretching 25 times, the obtained PBO fiber tow immediately enters the coagulation bath containing 15% phosphoric acid and the temperature is 25 ℃, A...

Embodiment 3

[0023] 4,6-diaminoresorcinol-terephthalate, polyphosphoric acid and P 2 o 5 According to the weight ratio of 1:6:3, add it into the pre-condensation reactor, stir at 80°C for 2 hours, then raise the temperature to 150°C within 3 hours and react for 5 hours, then raise the temperature to 180°C and react for 2 hours, the obtained PBO The slurry enters into the twin-screw reaction extruder with 105mm, aspect ratio of 60, rotating speed of 200 rpm, and temperature of 190°C. ℃, the size of the spinneret is 0.23×100 holes, passing through a tunnel with a length of 3.5 meters and a temperature of 80°C, the atmosphere in the tunnel contains H 3 PO 4 0.12g / L, side blowing speed 0.5 m / s, spinning speed 150 m / min, nozzle stretched 30 times, the obtained PBO fiber tow immediately enters the coagulation bath containing 25% phosphoric acid and the temperature is 40 ℃, After leaving the coagulation bath, the tow is dissolved in 10 g / L NH 3 After soaking in 8 g / L potassium hydroxide so...

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Abstract

The invention discloses a new method for preparing poly-p-phenylene benzobisoxazole fibers, which comprises the following steps: (1) The ratio of adding components to a precondensation reactor is: 1:1.5~6:0.7~3 4,6-diaminoresorcinol-terephthalate, polyphosphoric acid and P 2 o 5 , at 80-180°C, carry out the pre-condensation reaction in stages for 8-15 hours; (2) The pre-condensation polymer obtained in step (1) enters the twin-screw extruder to continue the reaction to obtain an inherent viscosity of 20-20. 40dl / g poly-p-phenylene benzobisoxazole slurry; (3) After the slurry obtained in step (2) is continuously squeezed into the spinning assembly, the coagulation process is first stretched, and then washed with alkali, washed with water, dried, Wind spinning poly-p-phenylene benzodiaxazole fiber. The invention has the advantages of low equipment requirements, short reaction period, high strength and modulus of the prepared fiber, simple process and controlled sewage discharge.

Description

technical field [0001] The invention relates to a method for preparing fibers, in particular to a method for preparing poly-p-phenylenebenzobisoxazole fibers. Background technique [0002] Poly-p-phenylene benzobisoxazole fiber (PBO) is a high-strength, high-modulus fiber, which is far superior to aramid fiber in terms of heat resistance and flame retardancy, and it has a good size Stability and chemical stability, it is favored in high-performance fiber composite materials, protective clothing, aviation and other fields. [0003] The preparation of PBO fiber basically adopts 4,6-diaminoresorcinol hydrochloride (DAR hydrochloride) to remove hydrogen chloride, and then carry out polycondensation reaction with terephthalic acid in polyphosphoric acid solvent system to prepare PBO slurries are then carried out by dry-jet wet spinning, and U.S. Patent Nos. 5,534,205 and 5,296,185 (The DowChemical Company) report the manufacture method of PBO fibers, but this method needs to rem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/74D01D5/098
Inventor 刘兆峰胡祖明潘婉莲尤秀兰于俊荣陈蕾诸静
Owner DONGHUA UNIV
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