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Polybenzoxazole-polyparaphenylenebenzodiimidazole O-PBI liquid crystal copolymer and preparation and application thereof

A technology of polybenzoxazole and benzodiimidazole, applied in the direction of single-component synthetic polymer rayon, textiles and papermaking, fiber chemical characteristics, etc., can solve complex process, lack of easy photodegradation performance and improvement, preparation To avoid problems such as long process, achieve good spinnability and heat resistance, facilitate industrialization, and excellent rheological properties

Inactive Publication Date: 2019-05-31
ZHEJIANG DINGLONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] 1) The process of manufacturing ABAA is complicated, the production capacity is low, and the expansion of application is limited due to high price
[0015] Due to the long preparation process and complicated process, the price of AB-type monomer is relatively high, and the price reduction of the prepared PBO fiber is not large, and it is difficult to reach 1800 yuan / kg or below: it can only be used for special occasions of national defense and military industry, especially for It is more suitable for the preparation of co-condensation composite fibers that need to ensure the integrity of PBO chain links, and cannot meet the urgent needs of cost-effective expansion applications in industrial and civil fields
[0016] 2) The lack and improvement of the photodegradable performance caused by the oxazole ring structure of PBO itself
Moreover, since formula (7) adopts the preparation method of TAB hydrochloride and XH-TA mixed polycondensation, a large amount of HCl gas is released during the process, and the material requirements of industrial equipment are very harsh, so it is urgently needed to replace the above with HCl-free monomers. Facilitate the implementation of industrialization

Method used

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  • Polybenzoxazole-polyparaphenylenebenzodiimidazole O-PBI liquid crystal copolymer and preparation and application thereof
  • Polybenzoxazole-polyparaphenylenebenzodiimidazole O-PBI liquid crystal copolymer and preparation and application thereof
  • Polybenzoxazole-polyparaphenylenebenzodiimidazole O-PBI liquid crystal copolymer and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] The preparation of embodiment 1 compound salt monomer TATAB (1,2,4,5-tetraaminobenzene of terephthalic acid)

[0063]

[0064] Add 200g deoxygenated water and 10.697g Na 2 CO 3 (0.1009mol) and 8.384g (0.0504mol) terephthalic acid (TA), stirring and heating up to 70°C until it dissolves into a light brown transparent solution, under the protection of nitrogen, add 14.34g (0.0505mol)1,2, 4,5-Tetraaminobenzene hydrochloride (TABH), after the addition was completed, stirred at 70-80°C for 15 minutes, then slowly cooled to room temperature, filtered, and the wet filter cake was washed with 30mL deoxygenated water, filtered and dried, and vacuum-dried at 70°C to obtain 12.80 g (0.0421 mol) of 1,2,4,5-tetraaminobenzene compound salt (TATAB) of terephthalic acid, the yield as TA is 83.35%. FT-IR (KBr) see attached figure 1 .

Embodiment 2

[0065] Example 2 O 4 -PBI (poly-2,5-benzoxazole-p-phenylenebenzimidazole) and its monofilament fibers

[0066]

[0067] A) poly-2,5-benzoxazole-p-phenylenebenzimidazole (2:1)O 4 -PBI

[0068] Sequentially add P into the glass polymerization reaction column 2 o 5 Mass concentration is 85.3% polyphosphoric acid (PPA) 18.0g and P 2 o 5 3.40g, turn on the spiral stirring, and raise the temperature to 100°C and control the speed of 350r / min to stir for 30min and wait for P 2 o 5 After the reaction was dissolved, pass N 2 Slowly add 2.45g of AHBA and 2.449g of TATAB (mol ratio 2:1, mass ratio 0.50:0.50) in sequence under protection for 3 minutes. After the addition, slowly rise to 172°C with stirring for 60 minutes. Light purple fluorescence appears, and keep warm at 172-178°C React for 20 minutes until the bronze-colored liquid crystal is filamentous. When the rotation speed drops significantly to 320r / min or below, the polymerization reaction is over, and the stirring ...

Embodiment 3

[0071] Example 3 O 3 -PBI (poly-2,6-benzoxazole-p-phenylenebenzimidazole) and its monofilament fibers

[0072]

[0073] A) poly-2,6-benzoxazole-p-phenylenebenzimidazole (1:1)O 3 -PBI

[0074] Sequentially add P into the glass polymerization reaction column 2 o 5 Mass concentration is 85.3% polyphosphoric acid (PPA) 18.0g and P 2 o 5 3.40g, turn on the spiral stirring, and raise the temperature to 100°C and control the speed of 350r / min to stir for 30min and wait for P 2 o 5 After the reaction was dissolved, pass N 2 Slowly add 3.256g of TATAB and 1.639g of HABA (mol ratio 1:1, mass ratio 0.665:0.334) sequentially under protection for 3 minutes, light brown fluorescence appears when the temperature rises slowly to 180°C under stirring for 40 minutes after addition, keep warm at 177-182°C React for 15 minutes until the bronze-colored liquid crystal is filamentous, and when the rotation speed drops significantly to 320r / min or below, the polymerization reaction is ove...

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Abstract

The invention discloses a polybenzoxazole-polyparaphenylenebenzodiimidazole O-PBI liquid crystal copolymer and preparation and application thereof. The polybenzoxazole-polyparaphenylenebenzodiimidazole O-PBI liquid crystal copolymer has a structure shown as the formula (I) and an intrinsic viscosity of 8-13 dl / g; in the formula (I) shown in the description, m and n represents numbers of corresponding molecular chain segments, and m / (n+m) ranges from 30% to 70%. The polybenzoxazole-polyparaphenylenebenzodiimidazole O-PBI liquid crystal copolymer is prepared through a following reaction formulashown in the description. The invention provides application of the polybenzoxazole-polyparaphenylenebenzodiimidazole O-PBI liquid crystal copolymer in the preparation of O-PBI fibers. The polybenzoxazole-polyparaphenylenebenzodiimidazole O-PBI liquid crystal copolymer helps evidently improve spinnability of PBI; no corrosive gas is produced during preparation, polymerization speed is high, productivity is high, and implementing is convenient; the prepared O-PBI fibers have good light resistance and heat resistance.

Description

technical field [0001] The invention relates to a kind of polybenzoxazole-p-phenylene benzodiimidazole O-PBI liquid crystal copolymer and its preparation and application. Background technique [0002] Since 1998, PBO fiber has been exclusively produced by Japanese Toyobo Company according to formula (1) polycondensation and spinning monopoly (trade name Zylon). It is mainly sold to Europe, America and Japan as military supplies, and the price is as high as 3,000 yuan / kg. [0003] [0004] Due to the difficulty in the source of the monomer 4,6-diaminoresorcinol hydrochloride (DARH), the HCl removal time of the process of formula (1)>30h, and the complicated semi-continuous polymerization operation, the industrialization process is extremely difficult. Although Toyobo company also adopts the patented technology of making compound salt TDH first and then preparing PBO fiber by self-condensation polymerization, it does not need to remove HCl and obtain higher molecular wei...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/22D01F6/78
Inventor 陈汉庚胡晓锋陈国泉金宁人
Owner ZHEJIANG DINGLONG TECH
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