A metal-organic framework nanosheet composite film and its preparation method and application

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: 2021-11-19
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A metal-organic framework nanosheet composite film and its preparation method and application

Examples

Experimental program
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example 1

[0030] Example 1 Preparation of ZIF-90 nanosheet PVDF composite membrane and study on gas separation performance

[0031] Preparation of ZIF-90 nanosheets: Dissolve 0.5772g imidazole-2-carbaldehyde and 0.2628g sodium formate in 30mL anhydrous methanol, stir magnetically until the solution becomes clear, and prepare solution A; dissolve 0.1346g anhydrous zinc chloride in 10mL Anhydrous methanol was prepared into solution B; the clarified solution A was slowly added to solution B, and the solution was mixed uniformly by electromagnetic stirring at the same time, and the ZIF-90 synthesis solution was prepared; finally, the ZIF-90 synthesis solution was put into the autoclave 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 h.

[0032] Take ZIF-90 and disperse it in n-hexane, the concentration is 1mg / mL, first (1) use liquid nitrogen to cool it down to -170 ℃ to completely freeze, (2) heat it to ...

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 The ultrasonic emulsifier was sonicated for 5 minutes and then transferred to the PTFE lining. After cooling at room temperature, 1.6 mL of hydrofluoric acid (HF) was slowly added. After stirring evenly, it was placed in a stainless steel hydrothermal reactor with a PTFE lining. , put it in an oven pre-heated to 150°C, react at a high temperature for 10h, lower the temperature to 80°C overnight (12h), and then heat up to 150°C for 10h. Turn off the oven and wait for it to slowly cool to room temperature in the oven, then take it out, wash it with DMF, methanol, and deionized water at 60° C. to obtain MIL-53-Fe particles, which are dried for late...

example 3

[0042] Example 3 Preparation of CuBTC nanosheet PES composite membrane and study 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 for 15h at 110°C. The obtained crystals were washed with an aqueous ethanol solution with a volume ratio of 1:1, followed by drying at 60°C overnight and 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 for 5 minutes, (1) (2) repeat the two steps for 12 times, and get peeled CuBTC nanometers after melting. tablet dispersion.

[0044] Preparation of modified PVDF hollow fiber membrane: cut the PVDF h...

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Abstract

The invention discloses a metal-organic framework nanosheet composite film and its preparation method and application. The preparation method of the metal-organic framework nanosheet composite film is as follows: dissolving metal-organic framework particles in an organic solvent or its aqueous solution, Perform multiple times of alternating freezing-high temperature treatment to obtain a dispersed nanosheet dispersion; using a polymer film as a substrate, modifying the substrate by ammoniation or hydroxylation to obtain a modified substrate; then uniformly spread the metal-organic framework nanosheet dispersion on the surface of the modified substrate by means of spin drop coating for self-assembly, and then treat the self-assembled substrate at 40-150° C. for 4-16 hours, A metal-organic framework nanosheet composite film was obtained. The composite membrane of the invention has good stability and rigidity, and good gas separation effect.

Description

technical field [0001] The invention relates to a metal-organic framework nano-sheet ultra-thin composite membrane, a preparation method and application thereof, and belongs to the technical field of functional membrane preparation and separation application. Background technique [0002] Metal-organic frameworks (MOFs) have attracted widespread attention since the yaghi group reported in the 1990s. So far, more than 70,000 MOFs have been reported successively, which are used in gas adsorption and separation, sensing, and catalysis. , 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 new separation technology emerging rapidly, has the advantages of low energy consumption, low cost and green environmental protection in gas separation. The esse...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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