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Metal-organic framework nano-sheet composite film, preparation method and application thereof

A metal-organic framework and nanosheet technology, which is applied in the field of metal-organic framework nanosheet ultra-thin composite membranes and its preparation, can solve the problem of low flux and selectivity, high mass transfer resistance, and difficulty in achieving huge separation efficiency and selectivity. Breakthrough and other problems, to achieve the effect of increasing the degree of adhesion, enhancing stability and rigidity, and good gas separation effect

Active Publication Date: 2019-09-24
ZHEJIANG UNIV OF TECH
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  • Abstract
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  • Claims
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Problems solved by technology

[0003] Membrane separation, as a rapidly emerging new separation technology, has the advantages of low energy consumption, low cost, and environmental protection in terms of gas separation. However, the gas separation membranes commonly used in the market are polymer membranes. Due to their The essential feature is that it is difficult to achieve a huge breakthrough in separation efficiency and selectivity, that is, there is a trade-off effect. Therefore, in order to break through this bottleneck, many researchers introduce another high-efficiency selective separation layer
MOFs have also been introduced into the field of gas separation membranes in the past ten years, and have shown excellent separation performance. However, the existing MOF membrane materials, such as CuBTC series, ZIF series and MIL series, are mostly in-situ grown MOF structures, which are easy to obtain. Dense separation layer, however, the resulting separation layer is thicker and has greater mass transfer resistance, and the MOF membrane prepared on the cheap and easy-to-obtain organic substrate membrane shows lower flux and selectivity in gas separation. Sex is generally below 20

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  • Metal-organic framework nano-sheet composite film, preparation method and application thereof

Examples

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example 1

[0030] Example 1 Preparation of ZIF-90 Nanosheet PVDF Composite Membrane and Research on Gas Separation Performance

[0031] Preparation of ZIF-90 nanosheets: Dissolve 0.5772g imidazole-2-carbaldehyde and 0.2628g sodium formate in 30mL of anhydrous methanol, stir magnetically until the solution is clear, and prepare solution A; dissolve 0.1346g anhydrous zinc chloride in 10mL Anhydrous methanol is prepared into solution B; the clear solution A is slowly added to solution B, and the solution is mixed uniformly by electromagnetic stirring at the same time, and ZIF-90 synthetic liquid is prepared; finally, ZIF-90 synthetic liquid is put into a high-pressure reactor and The solvothermal reaction was carried out at 150°C, and the product ZIF-90 was generated after the reaction was carried out for 8 hours.

[0032] Take ZIF-90 and disperse it in n-hexane with a concentration of 1 mg / mL. First (1) use liquid nitrogen to cool it down to -170°C until it freezes completely, (2) heat it ...

example 2

[0036] Example 2 Preparation of MIL-53 Nanosheet PAN Composite Membrane and Study on Gas Separation Performance

[0037] Preparation of MIL-53-Fe nanosheets: Mix 0.41g ferric chloride hexahydrate, 1g terephthalic acid, 23g DMF (molar ratio 1.0:1.5:130.0), stir with a glass rod until the mixture is uniform and completely dissolved, 800W Ultrasonic emulsification machine for 5 minutes and transferred to the polytetrafluoroethylene liner, slowly add 1.6mL hydrofluoric acid (HF) after cooling at room temperature, stir evenly and put it into a stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene liner , put it into an oven that was pre-heated to 150°C, react at high temperature for 10h, then lower the temperature to 80°C overnight (12h), and then raise the temperature to 150°C for 10h. Close the oven and wait until it is slowly cooled to room temperature in the oven, then take it out, wash with DMF, methanol, and deionized water at 60°C to obtain MIL-53-Fe pa...

example 3

[0042] Example 3 Preparation of CuBTC nanosheet PES composite membrane and research on gas separation performance

[0043] Preparation of CuBTC nanosheets: 1.22g copper(II) nitrate trihydrate, 0.58g 1,3,5-benzenetricarboxylic acid, 0.58g deionized water and 13.135g ethanol were put into a beaker and stirred for 30 minutes. And put it into a steel-lined polytetrafluoroethylene autoclave at 110°C for 15h. The obtained crystals were washed with an aqueous ethanol solution with a volume ratio of 1:1, then dried at 60° C. overnight, and dried at 110° C. for one day. The CuBTC particles were dispersed in absolute ethanol, and the concentration of CuBTC was 1 mg / mL. First (1) use liquid nitrogen to cool it down to about -179°C until it is completely frozen, (2) heat it to about 80°C to melt and keep it for 5 minutes, (1) and (2) repeat the two steps 12 times, and after melting, the exfoliated CuBTC nano tablet dispersion.

[0044] The preparation of the modified PVDF hollow fiber ...

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Abstract

The invention discloses a metal-organic framework nano-sheet composite film, a preparation method and an application thereof. The preparation method of the metal-organic framework nano-sheet composite film comprises the following steps: dissolving metal-organic framework particles in an organic solvent or an aqueous solution thereof, and carrying out a plurality of alternating freezing-high-temperature treatment to obtain a stripped nano-sheet dispersion; taking a high molecular polymer film as a substrate, modifying the substrate by ammoniation or hydroxylation to obtain a modified substrate; then, uniformly spreading the metal-organic framework nano-sheet dispersion on the surface of the modified substrate in a rotating drop coating manner for self-assembly, and treating the self-assembled substrate at 40-150 DEG C for 4-16 hours to obtain the metal-organic framework nano-sheet composite film. The composite film of the invention has good stability and rigidity, and has good gas separation effect.

Description

technical field [0001] The invention relates to a metal-organic framework nanosheet ultra-thin composite film and its preparation method and application, belonging to the technical field of functional film preparation and separation application. Background technique [0002] Since the yaghi research group reported metal-organic framework materials (MOFs) in the 1990s, it has attracted widespread attention. So far, more than 70,000 MOFs have been reported successively. , drug capture, semiconductor and other fields have shown great application prospects. Due to its ultra-high specific surface area and adjustable pore size, it exhibits unprecedented excellent performance in the field of gas adsorption and separation. [0003] Membrane separation, as a rapidly emerging new separation technology, has the advantages of low energy consumption, low cost, and environmental protection in terms of gas separation. However, the gas separation membranes commonly used in the market are p...

Claims

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Application Information

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IPC IPC(8): B01D71/06B01D69/12B01D69/02B01D67/00B01D53/22
CPCB01D53/228B01D67/0079B01D69/02B01D69/12B01D71/06B01D2325/24
Inventor 李洋周雨薇张旭秦磊张国亮
Owner ZHEJIANG UNIV OF TECH
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