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MOF/PIM-1 in-situ crosslinked matrix membrane and preparation method thereof

A PIM-1, in-situ cross-linking technology, applied in separation methods, chemical instruments and methods, membrane technology, etc., can solve problems such as poor compatibility

Inactive Publication Date: 2019-11-12
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of MOF and PIM-1 in situ cross-linked matrix membrane and preparation method thereof, this method solves the problem of poor compatibility between traditional composite membrane fillers and polymers, the prepared composite membrane has high Permeability and Selectivity

Method used

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  • MOF/PIM-1 in-situ crosslinked matrix membrane and preparation method thereof
  • MOF/PIM-1 in-situ crosslinked matrix membrane and preparation method thereof
  • MOF/PIM-1 in-situ crosslinked matrix membrane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Example 1: Set up a reflux device containing a three-necked flask. In a nitrogen atmosphere, 3.4gTTSBI, 2gDCTB and 4.14g anhydrous K 2 CO 3 Put it into a three-necked flask, add 20ml of NMP, stir at room temperature for 3 minutes, then add 10ml of toluene, immediately put it in a 160°C oil bath for 40 minutes, pour the solution obtained after the reaction into 200ml of methanol, stir for 2 hours, and use a pore size of Suction filter with 0.45μm nylon membrane, dry the obtained filter cake at 60°C for 6h, then dissolve the dried powder in 100ml of chloroform, stir for 2h, centrifuge, dissolve the bottom precipitate in 400ml of methanol, stir After 2 hours, the PIM-1 powder was obtained by suction filtration, and finally washed twice with deionized water, acetone, and dioxane in sequence, and dried to obtain fluorescent yellow PIM-1 powder. Dissolve 0.72g of PIM-1 powder in 10ml of chloroform and sonicate for half an hour to obtain a viscous solution, pour the solution ...

Embodiment 2

[0031] Embodiment 2: set up the reflux device that contains three-necked flask, in nitrogen atmosphere, with 3.4gTTSBI, 2gDCTB and 4.14g anhydrous K 2 CO 3 Put it into a three-necked flask, add 20ml of NMP, stir at room temperature for 3 minutes, then add 10ml of toluene, immediately put it in a 160°C oil bath for 40 minutes, pour the solution obtained after the reaction into 200ml of methanol, stir for 2 hours, and use a pore size of Suction filter with 0.45μm nylon membrane, dry the obtained filter cake at 60°C for 6h, then dissolve the dried powder in 100ml of chloroform, stir for 2h, centrifuge, dissolve the bottom precipitate in 400ml of methanol, stir After 2 hours, the PIM-1 powder was obtained by suction filtration, and finally washed twice with deionized water, acetone, and dioxane in sequence, and dried to obtain fluorescent yellow PIM-1 powder. 0.81g 2-aminoterephthalic acid, 1.06gZrCl 4 , 5ml of formic acid and 50ml of DMF were mixed and dissolved, stirred at roo...

Embodiment 3

[0036] Embodiment 3: 0.81g2-aminoterephthalic acid, 1.06gZrCl 4, 5ml of formic acid and 50ml of DMF were mixed and dissolved, stirred at room temperature for 3 hours, then the solution was transferred to a reaction kettle, and heated in an oven at 120°C for 24 hours to obtain a reaction mixture, and the bottom centrifuged product obtained by centrifugation was washed 4 times with methanol , and then activated in a vacuum oven at 120 °C for 24 hours to obtain UiO-66-NH 2 . Take 0.7 g of UiO-66-NH 2 Put into DMF (50mL), then add monomer and catalyst for PIM-1 polymerization, including DCTB (1.0g, 5.0mmol), TTSBI (1.7g, 5.0mmol) and K 2 CO 3 (2.1 g, 10.0 mmol). The reaction was carried out at 70°C for 24h, and the cross-linked UiO-66-NH 2 The yellow mixture with PIM-1 which precipitated at the bottom of the flask was filtered and washed with methanol (twice) and acetone (twice) to remove any residual catalyst and unreacted monomer. The product was dispersed in chloroform to...

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Abstract

The invention discloses an MOF / PIM-1 in-situ crosslinked matrix membrane and a preparation method thereof. The preparation method for the MOF / PIM-1 in-situ cross-linked matrix membrane comprises the following steps: mixing and dissolving UIO-66-NH2, 1,4-dicyanotetrafluorobenzene, 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl-1,10-spirodiacid, potassium carbonate and DMF, carrying out a reaction at70-80 DEG C for 12-72 h, and subjecting the obtained reaction liquid A to post-treatment to obtain a crosslinked product; dissolving the obtained crosslinked product in chloroform to obtain a viscoussolution, then uniformly and smoothly laying the viscous solution in a film forming apparatus, carrying out drying at room temperature for 24-36 hours to obtain to obtained a finished film, and subjecting the finished film to post-treatment to obtain the target product, i.e., the MOF / PIM-1 in-situ crosslinked matrix membrane. The CO2 flux of the MOF / PIM-1 in-situ crosslinked matrix membrane of theinvention is nearly doubled; the CO2 / CH4 selectivity of the MOF / PIM-1 in-situ crosslinked matrix membrane is increased to 31.9 compared with 12.3 of a PIM-1 membrane and 12.5 of a UiO-66-NH2 / PIM blend membrane; and the CO2 / N2 selectivity of the MOF / PIM-1 in-situ crosslinked matrix membrane is increased to 54.2 compared with 18.7 and 17.3 of the above two membranes.

Description

[0001] (1) Technical field [0002] The invention relates to polymer separation membrane technology, in particular to the technology of introducing MOF to make mixed matrix membrane through in-situ cross-linking and PIM-1 reaction. [0003] (2) Background technology [0004] Compared with conventional separation technology, membrane separation technology has the advantages of high separation efficiency, high efficiency and energy saving, small loss, small footprint, and simple operation. In 2004, Peter Budd successfully developed a PIM (microporous polymer) material containing a spiro ring structure. The PIM (microporous polymer) membrane that has attracted much attention has the characteristics of high permeability, but its selectivity is average. At present, a variety of fillers and PIM-1 have been used to make composite membranes to improve selectivity, but affected by trade-off, the selectivity is increased while the permeability is reduced. [0005] (3) Contents of the in...

Claims

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Application Information

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IPC IPC(8): B01D69/12B01D71/76B01D67/00B01D53/22
CPCB01D53/228B01D67/0006B01D69/125B01D71/76
Inventor 张国亮欧阳世文徐泽海孟琴
Owner ZHEJIANG UNIV OF TECH
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