Metal-organic framework membrane and preparation method thereof

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

Active Publication Date: 2018-10-26
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 membrane and preparation method thereof
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  • Metal-organic framework membrane and preparation method thereof

Examples

Experimental program
Comparison scheme
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 was 220 °C, the hot-pressing pressure was 0.2 MPa, and the hot-pressing time was 25 min. 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 model...

Embodiment 2

[0056] Mix metal source (zinc nitrate hexahydrate) with organic ligand (2-aminoterephthalic acid) and additive (polyvinyl alcohol, molecular weight 16000) evenly. Among them, relative to 1 mol of organic ligand, the amount of metal source is 1 mol, and the amount of polyvinyl alcohol is 0.001 mol. Spread it evenly on the base nickel foam (4cm*4cm), and heat press. The hot-pressing temperature was 85 ℃, the hot-pressing pressure was 0.2 MPa, and the hot-pressing time was 120 min. 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: Bruker D8 Advance, test int...

Embodiment 3

[0059] Mix metal source (cobalt nitrate hexahydrate) with organic ligand (benzimidazole) and additive (polyvinylpyrrolidone, molecular weight 40000) evenly. Among them, 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 was 120 °C, the hot-pressing pressure was 0.2 MPa, and the hot-pressing time was 70 min. 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: Bruker D8 Advance, t...

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Abstract

The invention discloses a method for preparing a metal-organic framework film. The method comprises: contacting a metal source with an organic ligand and forming a metal-organic framework film on a substrate by a hot pressing method. The method of the present invention can more conveniently and quickly obtain a large amount of metal-organic framework membranes with high purity, realize industrial production and application, and has the advantages of low cost, simple operation, rapid production, batch production and high purity.

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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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/58C07D235/06C07C229/76C07C227/18
CPCC07C227/18C07C229/76C07D233/58C07D235/06B01D71/028C07F1/00C07F3/003B01D2323/10B01D53/02B01D2253/204B01J20/226B01J20/28033B01D67/0079B01D2323/081B01D2323/08B01D71/022B01D71/48B01D71/62
Inventor 韩若丹
Owner 理工清科(北京)科技有限公司
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