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A self-polymerized microporous polyimide gas separation membrane and its preparation method and application

A technology of gas separation membrane and polyimide, applied in separation methods, semi-permeable membrane separation, dispersed particle separation, etc., can solve the problem of low gas flux, achieve high selectivity, good thermal stability and mechanical properties Effect

Active Publication Date: 2021-08-13
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, as a gas separation membrane, polyimide has excellent gas selectivity, but the gas flux is low

Method used

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  • A self-polymerized microporous polyimide gas separation membrane and its preparation method and application
  • A self-polymerized microporous polyimide gas separation membrane and its preparation method and application
  • A self-polymerized microporous polyimide gas separation membrane and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]

[0042] (1) In a nitrogen atmosphere, 9 ml of a mixed solvent of tetrahydrofuran / trifluoroacetic acid (V:V=1:2) was added to a round-bottomed flask containing 1.5282 g of 2-naphthol. 0.3076 g of glyoxal was added dropwise under stirring, and after the resulting mixture was reacted at room temperature for 3 hours, saturated NaHCO was added thereto. 3 aqueous solution, adjust pH=7, and quench the reaction. After that, it was extracted three times with dichloromethane (30 mL×3), the organic phase was separated and dried over anhydrous sodium sulfate, and the solvent was removed by rotary evaporation to obtain a crude product. Finally, column chromatography [SiO 2 , V (petroleum ether): V (dichloromethane) = 6: 1] separated to obtain white cotton wool needle-like five-membered epoxy hetero-bridged naphthalene ring structure monomer (7a, 14c-dihydronaphtho[2,1-b ]naphtho[1',2':4,5]furo[3,2-d]furan), the yield was 70%;

[0043](2) Suspend and dissolve 2 grams of white ...

Embodiment 2

[0046]

[0047] (1) In a nitrogen atmosphere, 9 ml of a mixed solvent of tetrahydrofuran / trifluoroacetic acid (V:V=1:2) was added to a round-bottomed flask containing 0.995 g of 2-naphthol. 0.576 g of 1,1,3,3-tetramethoxypropane was added dropwise with stirring, and after the resulting mixture was reacted at room temperature for 3 hours, saturated NaHCO was added thereto. 3 aqueous solution, adjust pH=7, and quench the reaction. After that, it was extracted three times with dichloromethane (30 mL×3), the organic phase was separated and dried over anhydrous sodium sulfate, and the solvent was removed by rotary evaporation to obtain a crude product. Finally, column chromatography [SiO 2 , V (petroleum ether): V (methylene chloride) = 6: 1] to separate and obtain the white six-membered epoxy hetero-bridge naphthalene ring structure monomer (16H-8,16-methyl dinaphtho[2,1-d :1',2'-g][1,3]dioxocane), the productive rate is 87%;

[0048] (2) Suspend and dissolve 2 grams of whit...

Embodiment 3

[0052] (1) Under a nitrogen atmosphere, add 12 milliliters of m-cresol in a three-necked round-bottomed bottle with 0.85 gram of A monomer, add 1.11 grams of 6FDA after completely dissolving, add 0.7 milliliters of isoquinoline after completely dissolving, and heat up to React at 80°C for 4 hours, then raise the temperature to 180°C for 12 hours. After the viscous reaction liquid was cooled to room temperature, the fibrous polymer was obtained by precipitation in methanol solution, and the obtained polymer was vacuum-dried at 100° C. for 12 hours after washing for 4 times. Obtain A-6FDA polymer with a yield of 94%; A-6FDA polymer structural formula is as follows:

[0053]

[0054] (2) 0.5 gram of A-6FDA polymer is dissolved in 6.25 milliliters of N-methylpyrrolidone (NMP), obtains 8% casting solution, after filtering, casting solution is poured on a clean horizontal glass plate, 80 °C for 12 hours to obtain a polymer film with a thickness of about 45 microns. At 35°C, the...

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Abstract

The invention relates to a self-polymerized microporous polyimide gas separation membrane and its preparation method and application, belonging to the technical field of membrane gas separation, in order to prepare and synthesize a polymer gas separation membrane with high selectivity and high permeability , to meet the requirements of practical industrial applications. In the present invention, the main chain of self-polymerized microporous polyimide contains a ladder structure, which increases the distance between polymer chains, facilitates the separation and diffusion of gases, and reduces the hydrogen bonds between polymer molecules. function, improve the solubility of the polymer, the present invention utilizes two kinds of diamines with ladder structure and dianhydrides with different structures to prepare through homopolymerization or copolymerization reaction. In the present invention, two kinds of ladder-shaped diamine monomers containing oxa-naphthalene structure were synthesized for the first time, and the trapezoidal self-polymerizing microporous polyimide polymer containing oxa-naphthene structure was synthesized through polycondensation reaction, which has good thermal stability and Mechanical properties, high selectivity to oxygen / nitrogen, can meet the practical application of gas separation.

Description

technical field [0001] The invention belongs to the technical field of gas separation by membrane method, and in particular relates to a self-polymerized microporous polyimide gas separation membrane and its preparation method and application. Background technique [0002] Energy shortage and environmental protection are major problems that need to be solved urgently in the world today, and they are also problems that need to be solved urgently in my country's socialist production and economic development. Gas separation membrane technology is an emerging "green technology", which has been widely concerned for its advantages of low energy consumption, simple equipment, convenient and flexible operation, etc. However, the gas separation performance of traditional membrane materials is not enough to meet the industrial requirements, so more and more researchers have begun to pay attention to new polymer membrane materials with high separation performance. [0003] Due to its ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/64B01D69/02B01D67/00B01D53/22
CPCB01D53/228B01D67/0006B01D69/02B01D71/64B01D2325/02
Inventor 李南文康拴艳
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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