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A kind of preparation method of poly-p-phenylene benzobisoxazole fiber

A technology of benzobisoxazole and polyparaphenylene, applied in the field of material science, can solve the problem of fiber polymerization degree (viscosity does not meet industrialization requirements, 4,6-diaminoresorcinol is unstable, unfavorable polymerization reaction and other problems, to achieve the effect of reducing equipment requirements, reducing polymerization time and high product purity

Active Publication Date: 2022-01-14
ZHEJIANG DINGLONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although many companies are currently researching the preparation method of PBO, there are still few companies with industrialized production. The main reason is that the main monomer used in PBO is 4,6-diaminoresorcinol (DAR) hydrochloride. In the early stage of polymerization, the monomer needs to remove hydrogen chloride gas at high temperature. There are two problems in the process of dehydrochlorination gas: (1) 4,6-diaminoresorcinol (DAR) is extremely unstable, and it encounters oxygen Rapid discoloration is oxidized, which is not conducive to the progress of polymerization; (2) the hydrogen chloride gas produced is very corrosive to equipment at high temperatures, which is one of the main reasons for restricting industrial production
In this study, the polymer was only prepared in PPA medium, and the intrinsic viscosity only reached 17, and the degree of polymerization (viscosity) of the obtained fiber did not meet the requirements of industrialization.

Method used

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  • A kind of preparation method of poly-p-phenylene benzobisoxazole fiber
  • A kind of preparation method of poly-p-phenylene benzobisoxazole fiber
  • A kind of preparation method of poly-p-phenylene benzobisoxazole fiber

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 20g (0.1mol) 4,6-dinitroresorcinol, 200ml methanol and 1.0g 5% palladium carbon (water content is 67.0%) in the autoclave of 500ml, seal the autoclave, nitrogen, hydrogen each replacement 5 Second, slowly raise the temperature to 45°C, pass hydrogen to 0.3MPa, keep it warm for 1.5h under this condition, raise the temperature to 55°C and 0.8MPa, continue to react until the pressure remains constant, continue to keep warm for 0.5h, stop the reaction, and take advantage of the nitrogen protection Heat to filter out the catalyst, add the filtrate dropwise to 20% phosphoric acid aqueous solution, stir fully, cool the filtrate to crystallize, filter to obtain off-white solid, use 0.5% tin protochloride methanol solution to beat the crude product, filter, and vacuum dry to obtain purity >99.5% of 4,6-diaminoresorcinol phosphate, the yield is 85.3%; its IR see attached figure 1 , 1 See attached for H-NMR figure 2 .

[0041] Add 14.0g 84.5% PPA and 8.5g P 2 o 5 , under...

Embodiment 2

[0043] Add 20g (0.1mol) 4,6-dinitroresorcinol, 200g of 4.5% aqueous sodium hydroxide solution and 2.0g Raney / Ni into a 500ml autoclave, seal the reaction vessel, and replace 5 times with nitrogen and hydrogen respectively. Slowly raise the temperature to 45°C, pass hydrogen to 0.3MPa, keep the temperature for 2.5h under this condition, raise the temperature to 55°C and 0.8MPa, continue the reaction until the pressure remains constant, continue to keep the temperature for 0.5h, stop the reaction, and filter while hot under the protection of nitrogen Remove the catalyst, cool the filtrate to 0-5°C, add 0.5g of stannous chloride to the filtrate, add 160g of 20% phosphoric acid dropwise under the protection of nitrogen, a white solid appears during the dropwise addition, and a large amount of solid precipitates after the dropwise, and the crude product is obtained by filtration , the crude product was beaten with 0.5% stannous chloride methanol solution, filtered, and vacuum-dried ...

Embodiment 3

[0046] Add 20g (0.1mol) 4,6-dinitroresorcinol, 180ml methanol and 1.2g 5% palladium carbon (water content is 67.0%) in the autoclave of 500ml, seal the autoclave, nitrogen, hydrogen each replacement 5 Second, slowly raise the temperature to 50°C, pass hydrogen to 0.5MPa, keep it warm for 1.5h under this condition, raise the temperature to 60°C and 1.0MPa, continue to react until the pressure remains constant, continue to keep warm for 0.5h, stop the reaction, and take advantage of the nitrogen protection. Heat to filter out the catalyst, add the filtrate dropwise to 20% phosphoric acid aqueous solution, stir fully, cool the filtrate to crystallize, filter to obtain off-white solid, use 0.5% tin protochloride methanol solution to beat the crude product, filter, and vacuum dry to obtain purity >99.5% of 4,6-diaminoresorcinol phosphate with a yield of 86.4%.

[0047] Add 14.0g of 84.5% PPA and 8.8g of PPA to the reaction flask 2 o 5 , under the protection of nitrogen, start sti...

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Abstract

The present invention relates to a kind of preparation method of poly-p-phenylene benzobisoxazole fiber, comprising the following steps: 4,6-diaminoresorcinol phosphate and terephthalic acid in polyphosphoric acid and phosphorus pentoxide In a mixed medium, under the protection of an inert gas, the polymerization reaction is carried out at 100-200°C to obtain poly-p-phenylenebenzobisoxazole. The present invention uses 4,6-diaminoresorcinol phosphate (DARP) to polymerize with terephthalic acid (TPA), which not only saves the time of dehydrochlorination gas, but also greatly reduces the requirements for equipment (no to remove hydrogen chloride).

Description

technical field [0001] The invention belongs to the technical field of material science, and in particular relates to a preparation method of poly-p-phenylene benzobisoxazole fiber. Background technique [0002] Poly(p-phenylene benzobisoxazole) fiber (PBO) was invented by the aerodynamic development researchers of the U.S. Air Force. The basic patent of polybenzoxazole was first owned by the Stanford University Research Institute (SRI), and later The American Dow (DOW) Chemical Company was authorized and carried out industrial development of PBO. At the same time, it improved the original monomer synthesis method. The new process has almost no isomer by-products, which improves the synthesis monomer yield. rate, laying the foundation for industrialization. [0003] PBO fiber has the advantages of good heat resistance, high strength and modulus, and is known as the super fiber of the 21st century. Since 1998, it has been exclusively produced by Toyobo Corporation of Japan ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/22D01F6/74C07C213/02C07C215/80
CPCC08G73/22D01F6/74C07C213/02C07C215/80
Inventor 潘志军金宁人顾峰雷戴学明
Owner ZHEJIANG DINGLONG TECH
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