Cross-linkable microporous polymer gas separation membrane and preparation method thereof

A microporous polymer, gas separation membrane technology, applied in separation methods, filtration separation, semi-permeable membrane separation, etc., can solve the problems of reduced selectivity of separated gases, solubility restriction, poor solubility, etc., and achieve mild reaction conditions. , low price, high efficiency of synthesis reaction

Inactive Publication Date: 2017-11-03
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since chain-like microporous polymers (PIMs) and most functionalized polymers only have good solubility in common non-polar solvents such as tetrahydrofuran and chloroform, but in polar solvents , such as N,N-dimethylformamide and N-methylpyrrolidone show poor solubility. Therefore, the problem of solubility restricts its further modification in the experimental process, especially in the process of industrial spinning application in
[0004] At the same time, under high pressure conditions, compressible gases, such as propylene / propane and carbon dioxide / methane, have a certain plasticizing effect on this type of polymer, resulting in a greatly reduced selectivity for separating gases.

Method used

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  • Cross-linkable microporous polymer gas separation membrane and preparation method thereof
  • Cross-linkable microporous polymer gas separation membrane and preparation method thereof
  • Cross-linkable microporous polymer gas separation membrane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Synthesis of polymer: under the protection of nitrogen atmosphere, the monomer CH 3 - TTSBI (3.684g, 0.01mol), TFTPN (2.001g, 0.01mol) and K 2 CO 3 (3.45g, 0.025mol) was dissolved in a mixed solvent of 18mL N,N-dimethylacetamide (DMAc) and 9mL toluene, stirred mechanically, and reacted at 150°C for 5 hours, then poured the viscous solution slowly Put into methanol, filter with suction to obtain a bright yellow fibrous polymer, then wash the polymer with methanol and distilled water for 3-5 times, and dry at 120° under vacuum to constant weight to obtain a yellow fluorescent polymer PIM-CH 3 , The conversion rate is 95%.

[0036] Its structural formula is as follows:

[0037]

[0038] (2) Preparation of brominated chain self-porous polymer membrane: 2.44g polymer PIM-CH 3 Dissolve in 250mL chlorobenzene, stir with magnetic force to form a homogeneous solution, add 1.82g N-bromosuccinimide and 0.16g azobisisobutyronitrile, react at 150°C for 5 hours, and precip...

Embodiment 2

[0048] (1) Synthesis of polymer: under the protection of nitrogen atmosphere, the monomer CH 3 - TTSBI (11.052g, 0.03mol), TFTPN (6.003g, 0.03mol) and K 2 CO 3 (11.04g, 0.08mol) was dissolved in a mixed solvent of 56mL N,N-dimethylacetamide (DMAC) and 11mL toluene, mechanically stirred, reacted at 160°C for 5 hours, and precipitated in methanol, followed by methanol and After washing with distilled water for 4 times, the polymer PIM-CH was obtained after filtration and drying 3 , The conversion rate was 93%.

[0049] Its structural formula is as follows:

[0050]

[0051] (2) Preparation of brominated chain self-porous polymer membrane: 7.3g polymer PIM-CH 3 Dissolve in 150mL chlorobenzene, stir with magnetic force to form a homogeneous solution, add 1.6g N-bromosuccinimide and 0.15g azobisisobutyronitrile, react at 130°C for 4 hours, and precipitate in methanol , after washing 4 times, filter and dry to obtain brominated polymer (bromination degree 50%).

[0052] Its...

Embodiment 3

[0061] (1) Synthesis of polymer: under the protection of nitrogen atmosphere, the monomer CH 3 - TTSBI (3.684g, 0.01mol), TTSBI (6.808g, 0.02mol), TFTPN (6.003g, 0.03mol) and K 2 CO 3 (12.4g, 0.09mol) was dissolved in a mixed solvent of 55mL N,N-dimethylacetamide (DMAC) and 14mL toluene, mechanically stirred, reacted at 160°C for 5 hours, precipitated in a large amount of methanol, and washed for 4 times, filter and dry to obtain the polymer CO-PIM-CH 3 -1, the conversion rate is 93%.

[0062] Its structural formula is as follows (n=0.33):

[0063]

[0064] (2) Preparation of brominated chain self-porous polymer membrane: 4.72g polymer CO-PIM-CH 3 -1 was dissolved in 47mL of chlorobenzene, stirred by magnetic force to form a homogeneous solution, added 1.2g of N-bromosuccinimide and 0.11g of azobisisobutyronitrile, and reacted at 150°C for 5 hours. Precipitate in the medium, wash 5 times, filter and dry to obtain brominated polymer (bromination degree 33%). Its struct...

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Abstract

A cross-linkable intrinsically-porous polymer gas separation membrane is characterized in that a structural general formula is shown in the specification, wherein 0<m<=1. The membrane has the advantages that raw materials are easy to obtain, operation is simple, conditions are mild and the gas separation membrane has good mechanical performance and high selectivity.

Description

technical field [0001] The invention relates to a gas separation membrane and a preparation method thereof, in particular to a cross-linkable microporous polymer (PIMs) gas separation membrane and a preparation method thereof. Background technique [0002] In 2004, Budd et al. synthesized a rigid chain-like self-porous polymer PIM1-6 with a twisted structure. Since its main chain cannot rotate freely, it can well hinder the effective accumulation between molecular chains and promote the formation of membranes. Continuous micropores are formed inside, and the obtained membrane material has good permeability and selectivity, showing certain advantages in gas separation. [0003] In recent years, a great deal of work has been reported on the improvement of gas separation performance by modifying the spiro-ring structure and functionalizing chain-like self-microporous polymers (PIMs). Among them, the classic one is that the introduction of tetrazole groups in the main chain str...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D53/22B01D71/72B01D67/00B01D69/08B01D39/02
CPCB01D39/02B01D53/22B01D69/08B01D69/125B01D71/72B01D2053/224B01D2323/30B01D2325/00
Inventor 李南文张淑芳和树庆王旭超刘磊
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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