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Metal organic framework film and preparation method therefor

A metal-organic framework and metal source technology, applied in the field of applied chemistry, can solve the problems of prone to membrane defects, long production cycle, and long reaction time, and achieve the effects of batch production, high purity, fast production, and simple operation

Active Publication Date: 2016-02-24
理工清科(北京)科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The in-situ growth method refers to directly putting the substrate for film formation into the reaction solution, and growing metal-organic framework crystals on the surface of the substrate. This method is simple to operate, but the reaction time is long, film defects are prone to occur, there are too many impurities, and it is difficult to expand the amount. Production; the LBL deposition method is to pre-modify the organic groups on the surface of the substrate first, and then place the substrate in the metal solution and the organic ligand solution in turn, and grow layer by layer to obtain a metal-organic framework film. The advantages of this method are simple operation, The product has high purity, but the processing time is long, and it is difficult to expand mass production; the seed crystal method is to pre-coat the seed crystal on the surface of the substrate, and then place it in the reaction solution to grow in situ to form a film. This method makes up for the in situ growth method to a certain extent. It is easy to have the defects of membrane defects and excessive impurities, but there are still relatively long reaction times compared with the present invention, and it is difficult to achieve mass production; the sonochemical method is a new method developed in recent years, which is achieved by placing the substrate The reaction solution is ultrasonically produced to produce metal-organic framework membranes. The advantage of this method is that the reaction conditions are mild (it can be carried out at room temperature), and the reaction is faster than other methods. However, its products often have a large number of defects, insufficient purity, and difficulty in mass production. Big
[0004] Generally speaking, the current preparation method has a long production cycle, insufficient batch production capacity, low yield, and high relative production cost, which needs to be improved urgently

Method used

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  • Metal organic framework film and preparation method therefor

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Mix metal source (anhydrous zinc acetate) with organic ligand (2-methylimidazole) and additive (polyethylene glycol, molecular weight 4000). Wherein, relative to 1 mol of organic ligand, the amount of metal source used is 0.1 mol, and the amount of polyethylene glycol used is 0.005 mol. Spread evenly on the base copper foil (4cm*4cm), hot press. The hot-pressing temperature is 220° C., the hot-pressing pressure is 0.2 MPa, and the hot-pressing time is 25 minutes. The metal-organic framework material is obtained on the base copper foil, and the metal-organic framework film is prepared.

[0054] The above materials were washed repeatedly with ethanol and dimethylformamide, and dried to obtain a purified metal-organic framework membrane. The metal-organic framework material loading on the film was 10.37 g / m2. In order to carry out X-ray powder diffraction and scanning electron microscope analysis on the metal organic framework film, wherein, X-ray powder diffraction mod...

Embodiment 2

[0056] Mix metal source (zinc nitrate hexahydrate) with organic ligand (2-aminoterephthalic acid) and additive (polyvinyl alcohol, molecular weight 16000) evenly. Wherein, relative to 1 mol of organic ligand, the amount of metal source used is 1 mol, and the amount of polyvinyl alcohol used is 0.001 mol. Spread it evenly on the base nickel foam (4cm*4cm), and heat press. The hot-pressing temperature is 85° C., the hot-pressing pressure is 0.2 MPa, and the hot-pressing time is 120 minutes. The metal-organic framework material is obtained on the base foamed nickel, and the metal-organic framework film is prepared.

[0057] The above materials were washed repeatedly with ethanol and dimethylformamide, and dried to obtain a purified metal-organic framework membrane. The MOF loading on the film was 6.03 g / m2. Carry out X-ray powder diffraction and scanning electron microscope analysis on the metal organic framework film, wherein, X-ray powder diffraction model: BrukerD8Advance, ...

Embodiment 3

[0059] Mix metal source (cobalt nitrate hexahydrate) with organic ligand (benzimidazole) and additive (polyvinylpyrrolidone, molecular weight 40000) evenly. Wherein, relative to 1 mol of organic ligand, the amount of metal source used is 0.01 mol, and the amount of polyvinylpyrrolidone used is 0.002 mol. Evenly spread on the base carbon cloth (4cm*4cm), hot press. The hot-pressing temperature is 120° C., the hot-pressing pressure is 0.2 MPa, and the hot-pressing time is 70 minutes. The metal-organic framework material is obtained on the base carbon cloth, and the metal-organic framework film is prepared.

[0060] The above materials were washed repeatedly with ethanol and dimethylformamide, and dried to obtain a purified metal-organic framework membrane. The MOF loading on the membrane was 8.06 g / m2. Carry out X-ray powder diffraction and scanning electron microscope analysis on the metal organic framework film, wherein, X-ray powder diffraction model: BrukerD8Advance, test...

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Abstract

The present invention discloses a method for preparing a metal organic framework film. The method comprises a step of contacting a metal source with an organic ligand to form the metal organic framework film on a substrate by a hot-pressing method. By means of the method provided by the present invention, a large number of metal organic framework films with quite high purity can be obtained conveniently and rapidly, so that industrialized production and application are implemented, and the method has the advantages of low costs, simplicity in operation, rapid production, mass production of products, high purity and the like.

Description

technical field [0001] The invention relates to the field of applied chemistry, in particular to a method for preparing metal-organic framework membranes. Background technique [0002] Metal-organic frameworks are a kind of crystalline porous materials, which are constructed by coordination between metal clusters or metal ions and organic ligands. They have the advantages of both inorganic and organic porous materials, with high specific surface area, orderly and repeatable channels, Rich functional groups, good stability, and diverse structures. Metal-organic framework membranes are one of the important application fields of metal-organic frameworks, and are widely used in gas separation, catalysis, sensors and many other fields. The preparation methods of metal-organic framework membranes mainly include in-situ growth method, LBL deposition method, seed crystal method, and sonochemical method. [0003] The in-situ growth method refers to directly putting the substrate fo...

Claims

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Application Information

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IPC IPC(8): C07D233/58C07D235/06C07C229/76C07C227/18
CPCC07C227/18C07C229/76C07D233/58C07D235/06B01D71/02232B01D67/0079B01D2323/08C07F1/00C07F3/003B01D2323/10B01D53/02B01D2253/204B01J20/226B01J20/28033B01D2323/081B01D71/62
Inventor 韩若丹
Owner 理工清科(北京)科技有限公司
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