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Polyimide aerogel fiber as well as preparation and application thereof

An aerogel fiber, polyimide technology, applied in the chemical characteristics of fibers, textiles and papermaking, one-component synthetic polymer rayon, etc. question

Active Publication Date: 2020-10-23
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of this method is complicated
Adding small molecules of triethylamine in the preparation process is difficult to completely remove, which may easily cause defects in the prepared airgel and cause environmental pollution.
On the other hand, nanofibers on the opposite side are difficult to disperse evenly during the dispersion process, and their partial aggregation is likely to cause defects in the prepared airgel material

Method used

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  • Polyimide aerogel fiber as well as preparation and application thereof
  • Polyimide aerogel fiber as well as preparation and application thereof
  • Polyimide aerogel fiber as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043](1) Under nitrogen protection, add 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl (TFMB, 6.4046g), 3,5-diaminobenzoic acid into a 250mL three-necked flask (DABA, 3.0229g) then add 150ml N-methylpyrrolidone (NMP), mechanically stir until TFMB and DABA are dissolved or evenly suspended in NMP, then add 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA , 17.7696g), after 36h of ice-water bath reaction, the temperature was raised to 190°C, and the reaction was carried out for 8h to obtain soluble polyimide. (Among them, 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl, Bid Pharmaceuticals, has a purity of 98%; 3,5-diaminobenzoic acid, Anaiji Chemical Reagent, has a purity of 98%; N-Methylpyrrolidone, Sinopharm Reagent, 98%; 4,4'-(Hexafluoroisopropene) diphthalic anhydride, Leyan Reagent, purity 97%)

[0044] (2) The spinning dope in step (1) is subjected to a wet spinning process, using water as a coagulation bath, the temperature is 10° C., the spinning speed is 5 m / min, ...

Embodiment 2

[0050] (1) Under nitrogen protection, add 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl (TFMB, 6.4046g), 3,5-diaminobenzoic acid into a 250mL three-necked flask (DABA, 3.0229g) then add 150ml N-methylpyrrolidone (NMP), mechanically stir until TFMB and DABA are dissolved or evenly suspended in NMP, then add 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA , 17.7696g), after 36h of ice-water bath reaction, the temperature was raised to 190°C, and the reaction was carried out for 8h to obtain soluble polyimide.

[0051] (2) The spinning dope in step (1) is subjected to a wet spinning process, using water as a coagulation bath, the temperature is 25°C, the spinning speed is 3m / min, and the winding speed is 5.5m / min.

[0052] (3) Place the polyimide fiber in step (2) in water for 48 hours to age.

[0053] (4) Place the polyimide fiber in step (3) in a freeze dryer, and freeze-dry at -80° C. and 20 Pa for 48 hours. That is, the polyimide airgel fiber is prepared.

[0054] ...

Embodiment 3

[0057] (1) Under nitrogen protection, add 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl (TFMB, 6.4046g), 2-(4-aminophenyl )-5-aminobenzimidazole (BIA, 2.1628g), then add 150ml N-methylpyrrolidone (NMP), mechanically stir until TFMB and DABA are dissolved or evenly suspended in NMP, then add 4,4'-(hexafluoro Isopropylene) diphthalic anhydride (6FDA, 17.7696g), after 36 hours of reaction in an ice-water bath, the temperature was raised to 190°C, and the reaction was carried out for 8 hours to obtain a soluble polyimide.

[0058] (2) The spinning dope in step (1) is subjected to a wet spinning process, using water as a coagulation bath, the temperature is 50° C., the spinning speed is 5 m / min, and the winding speed is 5.5 m / min.

[0059] (3) Place the polyimide fiber in step (2) in water for 48 hours to age.

[0060] (4) Place the polyimide fiber in step (3) in a freeze dryer, and freeze-dry at -80° C. and 20 Pa for 48 hours. That is, the polyimide airgel fiber is prepared.

[...

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Abstract

The invention relates to a polyimide aerogel fiber as well as preparation and application thereof, and the polyimide aerogel fiber is obtained by taking a binary anhydride and a diamine as raw materials through wet spinning and freeze drying. The method is simple to operate, environment-friendly in process and beneficial to large-scale production. The polyimide aerogel fiber material prepared by the method is high in strength and good in heat resistance, has excellent heat insulation and preservation characteristics, and can be widely applied to the field of preparation of various heat insulation and preservation.

Description

technical field [0001] The invention belongs to the field of organic airgel fiber and its preparation, in particular to a polyimide airgel fiber and its preparation and application. Background technique [0002] Airgel is a kind of continuous network porous material with low density, high specific surface area, high porosity and low thermal conductivity. Carriers and other fields have obvious application advantages, and are regarded as good substitutes for traditional foam materials. At present, there are various types of aerogels, mainly including silica, cellulose, carbon material aerogels, etc., and their chemical structure and microstructure have an important impact on their physical and chemical properties. Polyimide airgel materials have broad application prospects in aerospace, heat insulation protection, catalyst carriers and other fields due to their light weight, flexibility, high strength and high modulus, radiation resistance and unique high and low temperature ...

Claims

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Application Information

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IPC IPC(8): C08G73/10D01F6/78D01D5/06D01D5/12D01D10/02D01D10/06
CPCC08G73/1067C08G73/1042C08G73/1039C08G73/1085D01F6/78D01D5/06D01D5/12D01D10/02D01D10/06
Inventor 张清华李猛猛赵昕董杰张培炎甘锋郑森森
Owner DONGHUA UNIV
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