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Full-nano porous MOF/HOF composite film, preparation method and application thereof in gas separation

A nanoporous, gas separation technology, applied in semi-permeable membrane separation, separation method, dispersed particle separation, etc., can solve problems such as aging, affecting the stability of mixed matrix membrane, and easy plasticization of polymer matrix

Inactive Publication Date: 2020-12-18
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the traditional mixed matrix membrane has been greatly improved in terms of gas selectivity and permeability, the limitation of the performance of the polymer matrix on the performance of the final mixed matrix membrane is still a problem that needs to be solved when further improving the performance of the mixed matrix membrane. At the same time, the polymer matrix is ​​easy to plasticize and age, which also affects the stability of the mixed matrix membrane.

Method used

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  • Full-nano porous MOF/HOF composite film, preparation method and application thereof in gas separation
  • Full-nano porous MOF/HOF composite film, preparation method and application thereof in gas separation
  • Full-nano porous MOF/HOF composite film, preparation method and application thereof in gas separation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparation of ZIF-8: Weigh 1.17g zinc nitrate (Zn(NO 3 ) 2 ) and 22.7g of 2-methylimidazole (2-HmIm) in two beakers, ultrasonically dissolved and configured as an aqueous solution. The dissolved Zn(NO 3 ) 2 The solution was quickly mixed with the 2-HmIm solution, stirred magnetically at room temperature for 5 minutes, centrifuged (6500 rpm, 30 min) to collect the product, washed with deionized water, and finally dried at 60° C. for 10 hours to obtain dry activated ZIF-8 particles.

[0024] (2) Preparation of HOF precursor NBP-DAT: Add 8.16g tris(4-bromophenyl)amine, 10.43g 4-cyanophenylboronic acid and 284.61g anhydrous N,N-dimethyl to a three-necked reaction flask Formamide (DMF), nitrogen gas after sealing to exhaust the air. After 30 minutes, add 48mL, 0.275g·mL -1 K 2 CO 3 aqueous solution and 48mL deionized water, and continue to pass nitrogen protection. After 30 minutes, 1.56 g of tetrakis(triphenylphosphine) palladium was added, and finally heated to ...

Embodiment 2

[0031] (1) ZIF-8 particles are prepared in step 1 of Example 1;

[0032] (2) prepare NBP-DAT precursor according to embodiment 1 step 2;

[0033] (3) Preparation of MOF / HOF composite membrane: Weigh 9.6 mg of activated ZIF-8 particles into a 10 mL glass bottle, pipette 1 mL of anhydrous dimethyl sulfoxide (DMSO) into the glass bottle, and sonicate for 30 minutes , so that the ZIF-8 particles were evenly dispersed in the DMSO solution, and then accurately weighed 120 mg of HOF precursor NBP-DAT and dissolved in the above DMSO solution, and dissolved completely at 150°C as a composite membrane casting solution. Preheat the porous α-alumina substrate at 80°C for 30 minutes, pipette 100 μL of composite membrane casting solution and evenly drop-coat it on the preheated substrate, evaporate the solvent at 80°C, and obtain a homogeneous MOF / HOF after 2 hours The composite film is denoted as UPC-HOF-6 / ZIF-8-8, and the film thickness is 7.88 μm.

[0034] (4) Membrane characterization...

Embodiment 3

[0039] (1) ZIF-8 particles are prepared in step 1 of Example 1;

[0040] (2) prepare NBP-DAT precursor according to embodiment 1 step 2;

[0041] (3) Preparation of MOF / HOF composite membrane: Weigh 14.4 mg of activated ZIF-8 particles into a 10 mL glass bottle, pipette 1 mL of anhydrous dimethyl sulfoxide (DMSO) into the glass bottle, and sonicate for 30 minutes , so that the ZIF-8 particles were evenly dispersed in the DMSO solution, and then accurately weighed 120 mg of HOF precursor NBP-DAT and dissolved in the above DMSO solution, and dissolved completely at 150°C as a composite membrane casting solution. Preheat the porous α-alumina substrate at 80°C for 30 minutes, pipette 100 μL of composite membrane casting solution and evenly drop-coat it on the preheated substrate, evaporate the solvent at 80°C, and obtain a homogeneous MOF / HOF after 2 hours The composite film is denoted as UPC-HOF-6 / ZIF-8-12, and the film thickness is 10.77 μm.

[0042] (4) Membrane characterizat...

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Abstract

The invention discloses a full-nano porous MOF / HOF composite film, a preparation method and application of the film in gas separation, and belongs to the technical field of film materials and separation thereof. The preparation method comprises the following steps: synthesizing porous ZIF-8 particles with the particle size of about 100nm by adopting a hydrothermal method, uniformly dispersing different amounts of ZIF-8 in a UPC-HOF-6 casting solution by adopting an ultrasonic method, and obtaining a series of composite films with different composition proportions by adopting a solution casting-solvent evaporation method. The preparation method comprises the three steps of preparing the ZIF-8, preparing an HOF precursor NBP-DAT and preparing the MOF / HOF composite film. A scanning electron microscope result shows that the surface of the composite film is rough, particulate matters with different sizes exist, and the particulate matters are presumed to be doped ZIF-8 particles. A permeability comparison chart shows that the MOF / HOF composite films with different composition proportions have certain selectivity to H2 / N2, the gas permeability is increased and the separation selectivityis reduced along with the increase of the doping amount of the ZIF-8, so that the composite film disclosed by the invention can be used for gas separation.

Description

technical field [0001] The invention belongs to the technical field of membrane materials and separation thereof, and in particular relates to a full nanoporous MOF / HOF composite membrane, a preparation method and the application of the membrane in gas separation. Background technique [0002] Separation of gas molecules with similar physical or chemical properties is of industrial importance. The commonly used separation technique is cryogenic distillation, accounting for 90% to 95% of all isolates. But this technique is energy-intensive and difficult to separate gas molecules with similar compressibility and boiling points. Significant energy savings can be achieved by replacing energy-intensive distillation techniques with a relatively low-energy process. The new membrane separation technology has been widely studied in the field of gas separation due to its advantages of low energy consumption, simple operation, small footprint, and high efficiency, and has great poten...

Claims

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Application Information

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IPC IPC(8): B01D71/72B01D69/12B01D67/00B01D53/22C08G83/00
CPCB01D53/228B01D67/0002B01D69/12B01D71/72C08G83/008
Inventor 康子曦张彩艳范黎黎王荣明孙道峰
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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