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Support type ultrathin two-dimensional layered MOF film and preparation method thereof

A two-dimensional layered and supported technology, applied in the field of membrane separation, can solve the problems of damaged nanosheets, low yield of single-layer nanosheets, etc., and achieve high repeatability.

Active Publication Date: 2016-06-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yield of single-layer nanosheets obtained by delamination using this method is very low, and the intercalation agent needs to be completely removed before the obtained nanosheet materials can be used for subsequent research and use, such as the preparation of supported films, Washing steps are likely to damage the nanosheets or cause the nanosheet layers to restack and occlude each other with channels, resulting in a channelless block

Method used

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  • Support type ultrathin two-dimensional layered MOF film and preparation method thereof
  • Support type ultrathin two-dimensional layered MOF film and preparation method thereof
  • Support type ultrathin two-dimensional layered MOF film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1Zn2

[0039] Example 1Zn 2 (bim) 4 preparation of

[0040] 0.612 g of zinc chloride was dissolved in 23 ml of N,N-dimethylformamide (N,N-dimethylformamide, DMF), and stirred for 20 minutes. 0.354 g of benzimidazole was dissolved in another mixture of 23 ml of N,N-dimethylformamide and 0.22 g of diethylamine (DEA) and stirred for 20 minutes. The latter is then poured into the former solution while stirring. Zn 2 + / bim / DEA / DMF molar ratio is 1.5:1:1:200. Subsequently, the reaction liquid was transferred into a reaction kettle, and reacted at 130 degrees Celsius for 42 hours. The resulting reaction product was washed repeatedly with methanol, and finally put into an oven at 50°C to dry overnight.

[0041] X-ray diffraction confirmed that the product has a layered structure (such as figure 1 ), and its (002) characteristic peak appears near 9°. Scanning electron microscope pictures show that the particle size of the product is micron-scale, with obvious sharpened octahedral pri...

Embodiment 2

[0042] Example 2Zn 2 (bim) 4 preparation of

[0043] 3.025 g of zinc nitrate hexahydrate and 7.695 g of benzimidazole were added to 1000 ml of DMF, and stirred for 1 hour. Then the reaction solution was allowed to stand at room temperature for 72 hours. After the reaction, the ZIF-7 nanoparticles obtained by centrifugation were washed repeatedly with methanol, and the product was dried overnight in an oven at 50 degrees Celsius and then dried in a vacuum oven at 120 degrees Celsius for 48 hours.

[0044] The obtained ZIF-7 nanoparticles were dispersed in water at a concentration of 0.5 wt%, and refluxed at 100 degrees Celsius for 24 hours. After the suspension was filtered, the product was washed with deionized water and methanol, and finally dried overnight in an oven at 50°C. X-ray diffraction confirms that the product also has a layered structure (such as image 3 ), the product diffraction spectra obtained by the two methods can be well matched. The scanning electron...

Embodiment 3Zn2

[0045] Example 3Zn 2 (bim) 3 preparation of

[0046] 6 grams of zinc nitrate hexahydrate and 1.2 grams of benzimidazole were mixed and added to 100 milliliters of DMF, and the water bath was ultrasonically dissolved. Subsequently, the reaction solution was transferred to a reaction kettle, and reacted at 100 degrees Celsius for 72 hours. The reaction product was repeatedly centrifuged and washed with methanol, dried overnight at 60°C, and finally dried in a vacuum oven at 150°C for 24 hours. X-ray diffraction shows that the product is a layered crystal structure (such as Figure 5 ), the scanning electron microscope photo shows that this Zn 2 (bim) 3 The particles are diamond-like in shape, and the layered structure is obvious (such as Figure 6 ).

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Abstract

The invention relates to a support type ultrathin two-dimensional layered MOF film and a preparation method thereof. The preparation method comprises the steps of: (1) mixing a two-dimensional layered MOF material, anhydrous methanol and n-propanol in a mass ratio of 1:2000-5000:0-3000, then performing ball milling treatment at a speed of 30-200rpm for 30-200min; (2) standing the mixture obtained in step (1) for 4h-30d; and (3) under the condition of 20-200DEG C, dripping an upper solution obtained in step (2) to a porous base membrane carrier surface and conducting drying to obtain the product. The preparation method of the support type ultrathin two-dimensional layered MOF film provided by the invention can prepare a highly oriented support film without extra seed preparation and coating process and has high repeatability. The obtained support type ultrathin two-dimensional layered MOF film has excellent gas separation performance and wide application fields.

Description

technical field [0001] The invention belongs to the field of membrane separation, and relates to a high-performance supported ultrathin two-dimensional layered MOF membrane applied in the field of gas separation and a preparation method thereof. Background technique [0002] Energy saving and emission reduction technology is one of the keys to achieve sustainable development and environmental friendliness. The separation process accounts for 40% to 60% of the total energy consumption of the process industry, so the energy saving and emission reduction of the separation process has become one of the key concerns of global scientific researchers. Membrane separation has significant advantages such as low energy consumption, high separation efficiency, easy operation, and low carbon emissions. It can be used in many fields such as gas separation, seawater desalination, water pollution control, and pharmaceuticals. The gas separation membrane market is currently dominated by po...

Claims

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Application Information

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IPC IPC(8): B01D69/12B01D71/06B01D67/00
Inventor 杨维慎彭媛李砚硕
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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