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Technology for producing poly(p-phenylene benzobisoxazole) (PBO) fibers

A technology of benzobisoxazole and polyparaphenylene, which is applied in the chemical post-treatment of synthetic polymer artificial filaments, preparation of spinning solution, wet spinning, etc., can solve the problems of difficult control, complicated feeding procedures, and residence time To improve production efficiency, overcome difficulty in polymerization, and enhance stability

Active Publication Date: 2014-09-03
CHINA BLUESTAR CHENGRAND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 1. The feeding procedure is complicated. Since terephthalic acid (TPA) is insoluble in polyphosphoric acid (PPA), 1-10% TPA is added during the polymerization after the slurry, making it difficult to control the ratio of the two monomers in the polymerization;
[0008] 2. To fully mix the TPA slurry into the pre-polymerized material, it needs to stay for too long (more than 5h);
[0009] 3. Pre-polymerization conditions are harsh, monomer salts are easily oxidized and difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A process for producing poly-p-phenylene benzobisoxazole PBO fibers, comprising the following process steps:

[0049] A. Degassing, pre-polymerization and defoaming

[0050] Heat the polyphosphoric acid at 80°C for 60 minutes, then enter the degassing kettle, add 4,6-diaminoresorcinol hydrochloride, terephthalic acid and phosphorus pentoxide, and degas it in the degassing kettle After the degassing is completed, enter the mixing tank for pre-polymerization and degassing to obtain the pre-polymerized material;

[0051] B. Post-polymerization, defoaming

[0052] After the pre-polymerization is completed, the temperature of the mixing tank is raised to 110°C, and the pre-polymer material is pressed into the storage tank, and then the pre-polymer material is pressed into the screw extruder through a hydraulic press capable of precise flow control. The hydraulic press controls the output speed to be 10ml / min. The pre-polymer material is post-polymerized in the screw extrud...

Embodiment 2

[0060] A process for producing poly-p-phenylene benzobisoxazole PBO fibers, comprising the following process steps:

[0061] A. Degassing, pre-polymerization and defoaming

[0062] Heat the polyphosphoric acid at 120°C for 180 minutes, then enter the degassing kettle, add 4,6-diaminoresorcinol hydrochloride, terephthalic acid and phosphorus pentoxide, and degas it in the degassing kettle After the degassing is completed, enter the mixing tank for pre-polymerization and degassing to obtain the pre-polymerized material;

[0063] B. Post-polymerization, defoaming

[0064] After the pre-polymerization is completed, the temperature of the mixing tank is raised to 200°C, and then the pre-polymer material is pressed into the storage tank, and then the pre-polymer material is pressed into the screw extruder through a hydraulic press capable of precise flow control. The hydraulic press controls the output speed to be 100ml / min. The pre-polymer material is post-polymerized in the scre...

Embodiment 3

[0072] A process for producing poly-p-phenylene benzobisoxazole PBO fibers, comprising the following process steps:

[0073] A. Degassing, pre-polymerization and defoaming

[0074] Heat the polyphosphoric acid at 100°C for 120 minutes, then enter the degassing kettle, add 4,6-diaminoresorcinol hydrochloride, terephthalic acid and phosphorus pentoxide, and degas it in the degassing kettle After the degassing is completed, enter the mixing tank for pre-polymerization and degassing to obtain the pre-polymerized material;

[0075] B. Post-polymerization, defoaming

[0076] After the pre-polymerization is completed, the temperature of the mixing tank is raised to 155° C., and the pre-polymer material is pressed into the storage tank, and then the pre-polymer material is pressed into the screw extruder through a hydraulic press capable of precise flow control. The hydraulic machine controls the output speed to be 55ml / min, and the pre-polymer material is subjected to a post-polyme...

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PUM

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Abstract

The invention relates to a process for producing poly-p-phenylenebenzobisoxazole PBO fibers, belonging to the field of high-performance fiber production. The present invention solves the problem by optimizing equipment and control parameters through steps such as A, degassing, pre-polymerization and defoaming; B, post-polymerization, degassing; C, spinning, coagulation; D, post-processing; There are many problems in technology. The technical process, equipment coordination and control parameters in the basic technical scheme of the present invention are a complete system, which cooperate with each other and are indispensable, which can effectively transfer materials and realize the large-scale polymerization and subsequent large-scale spinning of PBO polymers. Get high quality PBO fiber products.

Description

technical field [0001] The invention relates to a production process of special fibers, more specifically, the invention relates to a process for producing poly-p-phenylene benzobisoxazole PBO fibers, belonging to the field of high-performance fiber production. Background technique [0002] PBO is the abbreviation of poly-p-phenylene benzobisoxazole. PBO fiber is a high-performance fiber made by spinning PBO polymer. Compared with other high-performance fibers, PBO fibers have higher specific strength, specific modulus, and heat-resistant and flame-retardant properties. They are known as "21st century super fibers" and are used to make high-performance composite materials, such as heat-resistant materials. , Anti-shock and anti-riot materials and structural stealth materials are widely used in high-tech fields such as aerospace, aviation and national defense. [0003] PBO polymers are usually prepared by polymerizing diaminoresorcinol hydrochloride (DAR) and terephthalic a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/94D01F1/10D01F11/08D01D1/02D01D1/10D01D5/06C08G73/22
Inventor 严家策范新年许伟郭玲赵亮钱军李欣欣
Owner CHINA BLUESTAR CHENGRAND CO LTD
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