Preparation method of triptyl polyimide separating film

A technology of pterene-based polyimide and separation membrane, which is applied in separation methods, semi-permeable membrane separation, dispersion particle separation, etc., to achieve the effects of increasing solubility, good self-stability, and improving stability

Active Publication Date: 2018-09-28
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, triptycene-based polymers, which are prepared by chemical dehydration to prepare

Method used

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  • Preparation method of triptyl polyimide separating film
  • Preparation method of triptyl polyimide separating film
  • Preparation method of triptyl polyimide separating film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Take 0.45g (1.5mmol) of 2,6,14-triaminotriptycene, put it into a 250ml flask, keep the temperature in an ice bath at about 0°C, then add 50ml of dimethylformamide to stir and dissolve, and add it in the form of powder 1.0 g (2.25 mmol) of hexafluorodianhydride was stirred and reacted for 6 hours under nitrogen protection. The ice bath was removed, 10 ml of acetic anhydride and 6 ml of pyridine were added thereto, and the reaction was stirred for 24 hours under nitrogen protection. After the reaction, configure 1L of methanol aqueous solution with a volume ratio of 1:1, pour the reaction product into the methanol aqueous solution, stir vigorously for 10 minutes, filter with suction, and dry the filter cake under vacuum at 50°C to obtain 0.9232g of Phenyl polyimide polymer.

[0039] Its structure is via 1 H-NMR and 1 C-NMR characterization confirmation, 1 H-NMR (500MHz, DMSO), δ=7.80-8.00ppm is the characteristic absorption peak of the H atom on the benzene ring of he...

Embodiment 2

[0043] Take 0.4g (1.34mmol) of 2,6,14-triaminotriptycene, put it into a 250ml flask, keep the temperature in an ice bath at about 0°C, then add 40ml of methylpyrrolidone to stir and dissolve, and add 0.52g in powder form (1.68mmol) 4,4'-biphenyl ether dianhydride, stirred and reacted for 8 hours under the protection of nitrogen. The ice bath was removed, 8 ml of acetic anhydride and 8 ml of triethylamine were added thereto, and the reaction was stirred for 24 hours under nitrogen protection. After the reaction, configure 1 L of methanol aqueous solution with a volume ratio of 1:1, pour the reaction product into the methanol aqueous solution, stir vigorously for 12 minutes, filter with suction, and dry the filter cake under vacuum at 60°C to obtain 0.6760 g of Phenyl polyimide polymer.

[0044] Its structure is via 1 H-NMR and 1 Confirmation by C-NMR characterization. 1 H-NMR (500 MHz, DMSO). δ=7.80-7.90ppm is the characteristic absorption peak of the H atom on the benzene...

Embodiment 3

[0048] Take 0.38g (1.27mmol) of 2,6,14-triaminotriptycene, put it into a 250ml flask, keep the temperature in an ice bath at about 0°C, then add 35ml of dimethylacetamide to stir and dissolve, and add it in the form of powder 0.5 g (1.55 mmol) of 3,3',4,4'-benzophenone tetracarboxylic dianhydride was stirred and reacted for 5 hours under nitrogen protection. The ice bath was removed, 6ml of acetic anhydride and 15ml of pyridine were added thereto, and the reaction was stirred for 36 hours under the protection of nitrogen. After the reaction, the reaction product was poured into methanol, vigorously stirred for 15 minutes, filtered with suction, and the filter cake was dried under vacuum at 70° C. to obtain 0.6120 g of triptyl polyimide polymer.

[0049] Its structure is via 1 H-NMR and 1 Confirmation by C-NMR characterization. 1 H-NMR (500 MHz, DMSO). δ=8.10-8.20ppm is the characteristic absorption peak of the H atom on the benzene ring of 3,3',4,4'-benzophenonetetracarbox...

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Abstract

The invention discloses a preparation method of a triptyl polyimide separating film. The preparation method comprises the following steps of dissolving a triptycene compound containing active groups and a dianhydride compound into a non-proton solvent to perform polymerizing reaction, and performing imidization treatment; pouring the obtained polymer solution after reaction into a settling solution, severely stirring, sucking and filtering, washing, and drying, so as to obtain triptyl polyimide powder; dissolving the triptyl polyimide into a solvent to obtain film casting liquid, coating a supporter with the film casting liquid, and drying, so as to obtain the triptyl polyimide separating film. The preparation method has the advantages that the problem of difficulty dissolving of the polyimide polymer is solved, and the limitation of application in the separating film is solved; by combining with the polyimide material, the thermal stability and chemical stability are good, the mechanical property is excellent, and the prepared triptyl polyimide separating film has better long-time stability.

Description

technical field [0001] The invention relates to a preparation method of a triptycene-based polyimide separation membrane, which belongs to the polymer membrane preparation technology and is suitable for the separation of mixtures of volatile organic compounds and air, such as in the field of oil and gas recovery. Background technique [0002] Volatile organic compounds are a class of substances with high volatility. Leakage will inevitably occur during its use, which will cause a large amount of volatile organic waste gas to be discharged into the atmosphere, affecting people's physical and mental health and polluting the environment. To this end, the country has promulgated various laws and regulations to control the emission concentration of volatile organic compounds, such as "Comprehensive Emission Standards of Air Pollutants". In order to meet the national emission requirements, researchers have developed a variety of technologies, such as using adsorption, absorption,...

Claims

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Application Information

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IPC IPC(8): B01D71/64B01D69/10B01D67/00B01D53/22
CPCB01D53/228B01D67/0011B01D69/10B01D71/64B01D2257/708
Inventor 周浩力戴山寅金万勤
Owner NANJING UNIV OF TECH
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