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Method for preparing polybenzazole fiber

A technology of phenylidene benzene and bisoxazole, which is applied in the field of polymer material preparation, can solve problems such as affecting the strength of the final product, incomplete closure of fiber holes, and increasing equipment load.

Inactive Publication Date: 2010-12-22
BEIJING TEX STRONG NEW MATERIAL DEV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] If a milder method is used for the acid washing process of the fiber, it will take a long time. If the method of lengthening the residence time of the fiber between the godet rollers is used, the load on the equipment will be increased; most of the existing patents use winding into a drum After soaking in water for a long time, this method is intermittent operation. Although it can remove phosphoric acid well, it is not conducive to maintaining the stability of production and controlling the uniformity of product quality.
If a more drastic method is used, such as neutralization with lye, due to the fast removal of phosphoric acid, the pores inside the fiber will not close completely, which will affect the strength of the final product

Method used

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  • Method for preparing polybenzazole fiber
  • Method for preparing polybenzazole fiber
  • Method for preparing polybenzazole fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The raw materials are diaminoresorcinol and terephthalic acid in a molar ratio of 1:1, and 0.5% stannous chloride antioxidant of the total mass of the raw materials is added to prepare the DAR compound salt. The pre-polymerization adopts a tank-type stirred reactor (made of 316L stainless steel) with a volume of 3 cubic meters. Gradually raise the temperature, and when the temperature reaches 90°C, start to add 60 kg of polyphosphoric acid, 30 kg of phosphorus pentoxide, 15 g of stannous chloride antioxidant, and 30 kg of DAR compound salt. Agitation was applied to the reactor during the addition. After the addition was completed, the temperature was continued to rise to 100° C., and the reaction was carried out for 10 hours, and the reactor was filled with nitrogen for protection. After the reaction is completed, open the channel connecting the lower part of the reactor to the inlet of the twin-screw extruder, increase the nitrogen pressure to 5 standard atmospheres, ...

Embodiment 2

[0049] Diaminoresorcinol and terephthalic acid are prepared according to the molar ratio of 1:1.1, and 1.2% stannous chloride antioxidant is added to prepare DAR compound salt. The pre-polymerization adopts a tank-type stirred reactor with a volume of 3 cubic meters. Gradually raise the temperature, and when the temperature reaches 100°C, start to add 91.5 kg of polyphosphoric acid, 45 kg of phosphorus pentoxide, 1500 g of stannous chloride antioxidant, and 12 kg of DAR compound salt. Agitation was applied to the reactor during the addition. After the addition was completed, the temperature was further raised to 110° C., and the reaction was carried out for 9 hours, and the reactor was filled with argon for protection. After the reaction is completed, open the channel connecting the lower part of the reactor to the inlet of the twin-screw extruder, increase the argon pressure to 6 standard atmospheres, and press the material into the screw extruder. The temperature of the sc...

Embodiment 3

[0051]Diaminoresorcinol and terephthalic acid are prepared according to the molar ratio of 1:0.9, and 0.1% stannous chloride antioxidant is added to prepare DAR compound salt. The pre-polymerization adopts a tank-type stirred reactor with a volume of 3 cubic meters and the upper part is filled with nitrogen. Gradually raise the temperature, and when the temperature reaches 120°C, start to add 41 kg of polyphosphoric acid, 50 kg of phosphorus pentoxide, 1000 g of stannous chloride antioxidant, and 8 kg of DAR compound salt. Agitation was applied to the reactor during the addition. After the addition was completed, the temperature was continued to rise to 120° C., and the reaction was carried out for 10 hours, and the reactor was filled with nitrogen for protection. After the reaction is completed, open the channel connecting the lower part of the reactor to the inlet of the twin-screw extruder, increase the nitrogen pressure to 7 standard atmospheres, and press the material in...

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Abstract

The invention relates to a method for preparing poly (p-phenylene) bis (benzoxazolyl) fibers, which belongs to the technical field of preparation of polymer materials. The method comprises the following steps: firstly, composite salt is prepared by diamino hydroxyphenol hydrochloride and a terephthalic acid, and phosphorus pentoxide, a polyphosphoric acid and an auxiliary agent are added into thecomposite salt, and subjected to prepolymerization under the condition of stirring and heating; secondly, a polymer reaction mixture after prepolymerization is over enters a screw extruder for further polymerization under the pressure of high-pressure inert gas or under the actuation of mechanical propulsion; thirdly, the polymer reaction mixture is extruded by the screw extruder, filtered, accurately measured, ejected, and solidified and formed in a solidification liquid after passing through a section of spinning shaft of inert gas; and fourthly, the polymer reaction mixture is subjected tofive procedures of a diluted phosphoric acid aqueous solution, water, hot water, an alkaline solution and purified water for cleaning and removal of a phosphoric acid, and dried, rolled and formed. The method completely removes the phosphoric acid; the process is tempered; drying under the condition of exertion of a tensile force helps to close fiber holes; and the products produced have high strength and modulus.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, in particular to a production process of poly-p-phenylene benzobisoxazole fiber. Background technique [0002] Poly-p-phenylene benzobisoxazole fiber, also known as poly-p-phenylene benzobisoxazole fiber, PBO fiber (Polybenzoxazole, hereinafter referred to as PBO fiber). PBO fiber has excellent characteristics such as high strength, high modulus, and high temperature resistance, and is used in heat-resistant industrial textiles and fiber reinforced materials. The chemical structure of PBO fiber is shown in the following two structural formulas. Wherein the theoretical modulus of the cis structure (as above) is higher than that of the trans structure (as below). [0003] [0004] The synthesis of PBO mostly uses polycondensation of 4,6-diaminoresorcinol hydrochloride (DAR hydrochloride) and terephthalic acid. The polymerization solvent is generally polyphosphoric acid (o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/74D01D1/02D01D5/06D01D10/06
Inventor 尹晔东赵国樑
Owner BEIJING TEX STRONG NEW MATERIAL DEV
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