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Poly(p-phenylene benzobisoxazole) fiber spinning forming method

A technology of benzobisoxazole and polyparaphenylene, which is applied in the directions of dry spinning, wet spinning, and fiber processing, can solve the problems of limiting fiber properties, limiting mechanical properties, and high phosphoric acid residues, and improving the fiber forming effect. , to eliminate the jitter of silk strips and increase the effect of dwell time

Active Publication Date: 2021-06-11
SHANDONG NON METALLIC MATERIAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The problem in the prior art is: the PBO fiber prepared by the conventional process has an obvious skin-core structure, which limits the further improvement of the fiber performance
This process shows that the coagulant in the coagulation bath diffuses to the inside of the PBO stock solution stream, and the solvent in the stock solution stream diffuses outward. However, due to the uneven dispersion of the coagulant in the PBO stock solution stream, the concentration of the coagulant on the surface is much higher than that in the interior, resulting in The surface layer is first solidified and oriented under the spinning tension to form a dense skin structure, but it is difficult to discharge the solvent inside the fiber, and the desolventization can only be completed in the subsequent washing or even drying process, so the structure is loose and the grains are large
The internal and external structure of the PBO fiber prepared by the conventional process is different, which limits the improvement of its mechanical properties, and because of the barrier of the skin layer, the internal phosphoric acid solvent is not easy to precipitate, and the final product has a high residual phosphoric acid and poor aging resistance. How to overcome the above difficulties has become a technology in the art. Problems that people need to solve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of spinning device of PBO fiber, its specific structure is as follows:

[0033]It consists of a prepolymerization tank, a twin-screw extruder, a melt pipeline, a metering pump, a spinneret and a solidification forming system connected in sequence, wherein the prepolymerization tank is set at the feed end of the twin-screw extruder, and the twin-screw extruder The discharge end is connected with a melt pipeline and a metering pump, and a spinneret is installed at the end of the melt pipeline, and the solidification forming system is located below the spinneret;

[0034] The specific structure of the solidification forming system is as follows:

[0035] It consists of two vertical coagulation baths: coagulation bath A and coagulation bath B in series, in which coagulation bath A is set under the spinneret, and a vertical spinning sleeve is arranged inside it, and a steady flow plate is installed at the entrance of the spinning sleeve , the bottom of the spinning s...

Embodiment 2

[0039] Utilize the spinning device of the PBO fiber described in embodiment 1, provide a kind of poly-p-phenylene benzobisoxazole fiber spinning forming method, comprise the steps:

[0040] (1) Add 500g of polyphosphoric acid solvent in a nitrogen-filled polymerization kettle, add 70.5g of polymerized monomer terephthaloyl chloride (TPC) and stir for 30min, add 1.2g of antioxidant stannous chloride, and heat up to 100°C , stirred for 30min, added 4,6-diaminoresorcinol hydrochloride (DAR·HCl) with a molar ratio of 0.85:1 to TPC, stirred for 10min, then added 162.2g of phosphorus pentoxide (P 2 o 5 ), stirred for 10 minutes, raised the temperature to 120°C, and stirred for 36 hours to complete the prepolymerization, and the intrinsic viscosity of the prepolymer was 0.4dl / g.

[0041] (2) The prepolymer is transported to the twin-screw extruder through pipelines, and at the same time, the third monomer ① with a molar ratio of DAR·HCl of 0.15:1 is added to the twin-screw extruder ...

Embodiment 3

[0046] Utilize the spinning device of the PBO fiber described in embodiment 1, provide a kind of poly-p-phenylene benzobisoxazole fiber spinning forming method, comprise the steps:

[0047] (1) Add 500g of polyphosphoric acid solvent in a nitrogen-filled polymerization kettle, add 97.6g of polymerized monomer terephthaloyl chloride (TPC) and stir for 60 minutes, add 1.8g of antioxidant stannous chloride, and heat up to 120°C , stirred for 60min, added 4,6-diaminoresorcinol hydrochloride (DAR·HCl) with a molar ratio of 0.95:1 to TPC, stirred for 20min, then added 189.3g of phosphorus pentoxide (P 2 o 5 ), stirred for 20 minutes, raised the temperature to 150°C, and stirred for 48 hours to complete the prepolymerization, and the intrinsic viscosity of the prepolymer was 1dl / g.

[0048] (2) The prepolymer is transported to the twin-screw extruder through pipelines, and at the same time, the third monomer ③ with a molar ratio of 0.05:1 to TPC is added to the twin-screw extruder i...

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Abstract

The invention belongs to the field of high-performance fibers, and particularly relates to a poly(p-phenylene benzobisoxazole) (PBO) fiber spinning forming method. The method comprises the following steps of firstly, preparing a low-viscosity PBO prepolymer, then conveying the prepolymer to a double-screw extruder, adding a third monomer into a polymerization system in a side feeding manner, and performing copolymerizing in the double-screw extruder to obtain a final spinning solution; and extruding the spinning solution from a spinneret plate, performing stretching in an air layer, then entering a coagulating bath tank, completing double diffusion, and perform coagulating to form fibers. The finally prepared PBO fibers are compact in structure, high in internal and external uniformity, good in mechanical property, low in phosphoric acid residual rate and more excellent in comprehensive performance.

Description

technical field [0001] The invention belongs to the field of high-performance fibers, and in particular relates to a poly-p-phenylenebenzobisoxazole (PBO) fiber spinning forming method. Background technique [0002] Poly-p-phenylenebenzobisoxazole (PBO) fiber is currently the best high-performance organic fiber with the best comprehensive properties. It has the characteristics of high strength, high modulus, high temperature resistance, and high flame retardancy. It is known as the super fiber of the 21st century. . PBO fibers can be used in cutting-edge fields such as national defense, aerospace, sports equipment, high-temperature filtration, and special protection. In the 1960s and 1970s, the Wright-Patteron Laboratory of the U.S. Air Force started the basic research on PBO fibers. In the 1990s, Dow Chemical Company cooperated with Japan Toyobo to develop PBO fibers. Subsequently, Toyobo succeeded in the pilot test and launched commercial products. Zylon. Afterwards, ma...

Claims

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Application Information

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IPC IPC(8): D01F6/78D01D5/04D01D5/06D01D5/34C08G73/22
CPCD01F6/78D01D5/04D01D5/06D01D5/34C08G73/22
Inventor 陈湘栋张殿波刘薇钟蔚华刘宗法郭程张晓光刘群孟昭瑞
Owner SHANDONG NON METALLIC MATERIAL RES INST
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