Preparation method of poly-p-phenylene benzobisoxazole fiber

A technology of benzobisoxazole and polyparaphenylene, applied in the field of polymer fiber preparation, can solve the problems of increased process difficulty, increased side reactions, and high requirements

Inactive Publication Date: 2011-11-30
SINOSELEN HI TECH
View PDF7 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. During the dehydrochlorination process of 4,6-diaminoresorcinol hydrochloride, a large amount of hydrogen chloride gas will be released, and these gases will generate a large amount of foam in the viscous reaction liquid, thereby reducing the agitation of the reaction system Efficiency; a large amount of foam produced makes 4,6-diaminoresorcinol hydrochloride adhere to the reactor wall, which easily destroys the balance of the ratio of polymer raw materials, thus making the final molecular weight of the prepared polymer poor in repeatability
[0006] 2. Hydrogen chloride is a strong corrosive gas, which makes the reaction have high requirements for equipment materials, and the degassing process takes a lot of time
[0007] 3. It is difficult to completely remove hydrogen chloride

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of poly-p-phenylene benzobisoxazole fiber
  • Preparation method of poly-p-phenylene benzobisoxazole fiber
  • Preparation method of poly-p-phenylene benzobisoxazole fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037]3117.4 grams of terephthalic acid and 1502.3 grams of sodium hydroxide were dissolved in 15000 grams of water to prepare an aqueous solution of sodium terephthalate with a concentration of 20.1 wt%. Under normal temperature, nitrogen atmosphere and stirring conditions, 4000 grams of solid powdery 4,6-diamino-1,3-resorcinol hydrochloride was added to the above-mentioned sodium terephthalate aqueous solution within 20 minutes, and the addition was completed. After that, the temperature of the system was raised to 80°C within 20 minutes, and a large amount of white precipitate appeared. The white precipitate was 4,6-diaminoresorcinol / terephthalic acid compound salt, and continued at 80°C The reaction was stirred for 30 minutes. Then filter, and weigh the filtered water removed, which is 13324 grams (accounting for 85% of the total water weight of the system); 2352 grams of water remain in the system. Under nitrogen protection, add 16170 grams of polyphosphoric acid and 138...

Embodiment 2

[0041] 3,117.4 grams of terephthalic acid and 1,502.3 grams of sodium hydroxide were dissolved in 21,500 grams of water to prepare an aqueous solution of terephthalic acid sodium salt with a concentration of 15.1 wt%. Under normal temperature, nitrogen atmosphere and stirring conditions, 4000 grams of solid powdery 4,6-diamino-1,3-resorcinol hydrochloride was added to the above-mentioned sodium terephthalate aqueous solution within 20 minutes, and the addition was completed. Afterwards, the temperature of the system rose to 80° C. within 20 minutes, a large amount of white precipitates appeared, and the stirring reaction was continued at 80° C. for 30 minutes. Filter, and weigh the filtrated water removed, which is 17741 grams (accounting for 80% of the total water weight of the system), and 4439 grams of water remain in the system. Under the protection of nitrogen, 21443 grams of polyphosphoric acid and 19299 grams of phosphorus pentoxide were added to the system, reacted at ...

Embodiment 3

[0045] 3117.4 grams of terephthalic acid and 1502.3 grams of sodium hydroxide were dissolved in 11155 grams of water, and the concentration of the prepared aqueous solution of sodium terephthalic acid salt was 25.0 wt%. Under normal temperature, nitrogen atmosphere and stirring conditions, 4000 grams of solid powdery 4,6-diamino-1,3-resorcinol hydrochloride was added to the above-mentioned sodium terephthalate aqueous solution within 20 minutes, and the addition was completed. Afterwards, the temperature of the system rose to 80° C. within 25 minutes, a large amount of white precipitates appeared, and the stirring reaction was continued at 80° C. for 30 minutes. Filter, and weigh the filtrated water removed, which is 10647 grams (accounting for 90% of the total water weight of the system), and 1184 grams of water remain in the system. Under nitrogen protection, 11424 grams of polyphosphoric acid and 9368 grams of phosphorus pentoxide were added to the system, and 1251 grams re...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
Thicknessaaaaaaaaaa
Apertureaaaaaaaaaa
Tensile strengthaaaaaaaaaa
Login to view more

Abstract

The invention relates to a preparation method of poly-p-phenylene benzobisoxazole fiber, which is an improvement to the existing salt-forming method. The present invention is that terephthalic acid and 4,6-diaminoresorcinol hydrochloride are neutralized by acid and alkali to directly generate 4,6-diamino-1,3-resorcinol/terephthalic acid composite salt, remove 80-90% of the water in the system by filtration, the compound salt does not need to be further washed and dried, and polyphosphoric acid and phosphorus pentoxide are directly added for polymerization to prepare a poly-p-benzobisoxazole prepolymer. Then the prepolymer is subjected to twin-screw continuous post-polymerization, filtration and defoaming, and directly enters spinning equipment for spinning, water washing, drying and winding to obtain poly-p-phenylene benzobisoxazole fibers. The invention can greatly save time, omit the hydrogen chloride removal process, and increase the continuity of the production process.

Description

technical field [0001] The invention relates to a preparation method of polymer fibers, in particular to a preparation method of poly-p-phenylene benzobisoxazole fibers. Background technique [0002] PBO fiber is the abbreviation of polyparaphenylene benzobisoxazole (PBO) fiber. The fiber has main performance indicators such as 5.8GPa tensile strength and 280GPa modulus, 68 LOI value and 650℃ decomposition temperature, and has good environmental stability, all of which belong to the current performance of organic and inorganic fibers. Most, its specific strength is about 12-14 times that of steel, its specific modulus is 1.4 times that of steel, and its specific gravity is 1.54-1.56g / cm 3 Only 1 / 5 of steel. Due to its superior performance, it has been regarded as a new generation of super fiber for the preparation of advanced structural composite materials in aerospace and military fields since its appearance. At present, PBO uses 4,6-diaminoresorcinol hydrochloride and te...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): D01F6/74C08G73/22
Inventor 侯庆华杨本森曹春朴连宏光
Owner SINOSELEN HI TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap