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Method for repairing defects of zif-67 film in situ and prepared film

A ZIF-67, in-situ repair technology, applied in the direction of superimposed layer plating, metal material coating process, coating, etc., can solve the problems of metal-organic framework membrane defects, insufficient separation ability of mixed gas, etc., to achieve fast and simple Factor of safety, reduction of input costs, effect of repairing surface defects

Active Publication Date: 2021-05-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the current situation that metal-organic framework membranes are prone to defects during the preparation process, and membrane defects will lead to insufficient separation ability for mixed gases

Method used

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  • Method for repairing defects of zif-67 film in situ and prepared film
  • Method for repairing defects of zif-67 film in situ and prepared film
  • Method for repairing defects of zif-67 film in situ and prepared film

Examples

Experimental program
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Effect test

Embodiment 1

[0030] The present embodiment is under the condition of electrification, does not add defect repairing agent, one-step preparation ZIF-67 thin film comprises the following steps:

[0031] (1) Soak the anodized aluminum substrate in water at 80°C for 1 hour, then soak it in acetone solution and wash it for 10 minutes. After drying, place it in a magnetron sputtering apparatus to spray gold on its surface. The gold spray current is 10mA. Gold spraying time is 3 minutes;

[0032] (2) Weigh and dissolve cobalt nitrate hexahydrate (0.58g) and 2-methylimidazole (0.33g) in 100mL methanol to obtain the precursor solution;

[0033] (3) Add the clarified solution of step (2) gained in the electrolytic cell, immerse the anodized aluminum substrate processed through step (1), and react for 15 minutes under a current of 1mA to obtain a defective ZIF-67 film.

[0034] The ZIF-67 film surface that step (3) obtains is carried out scanning electron microscope characterization, as figure 1 As...

Embodiment 2

[0037] In this embodiment, under the condition of energization, a defect repairing agent is added, (anhydrous zinc acetate and cobalt nitrate hexahydrate molar ratio is 0.01: 1), and a defect-free ZIF-67 film is prepared in one step, comprising the following steps:

[0038] (1) Soak the anodized aluminum substrate in water at 80°C for 1 hour, then soak it in acetone solution and wash it for 10 minutes. After drying, place it in a magnetron sputtering apparatus to spray gold on its surface. The gold spray current is 10mA. Gold spraying time is 3 minutes;

[0039] (2) Weigh and dissolve cobalt nitrate hexahydrate (0.58g) and 2-methylimidazole (0.33g) in 100mL methanol to obtain the precursor solution;

[0040] (3) Take by weighing 3.67 mg of anhydrous zinc acetate, add to the precursor solution described in step (2), and ultrasonically dissolve under an ice bath to obtain a clear solution;

[0041] (4) Add the clarified solution of step (3) gained in the electrolytic cell, imme...

Embodiment 3

[0045] In this embodiment, under the condition of energization, a defect repairing agent is added, (anhydrous zinc acetate and cobalt nitrate hexahydrate molar ratio is 0.02: 1), and a defect-free ZIF-67 film is prepared in one step, comprising the following steps:

[0046] (1) Soak the anodized aluminum substrate in water at 70°C for 2 hours, then soak it in acetone solution and wash it for 20 minutes. After drying, place it in a magnetron sputtering apparatus to spray gold on its surface. The gold spray current is 20mA. Gold spraying time is 2 minutes;

[0047] (2) Weigh and dissolve cobalt nitrate hexahydrate (0.87g) and 2-methylimidazole (0.49g) in 100mL methanol to obtain the precursor solution;

[0048] (3) Take by weighing 11 mg of anhydrous zinc acetate, add to the precursor solution described in step (2), ultrasonically dissolve under ice bath, obtain clear solution;

[0049] (4) Add the clarified solution obtained in step (3) into the electrolytic cell, immerse the ...

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Abstract

The invention discloses a method for in-situ repairing ZIF-67 film defects and the prepared film. The method comprises: processing an anodized aluminum substrate, preparing a precursor solution, adding a repair agent and in-situ repairing ZIF-67 film defects. In the present invention, by adding zinc acetate as a defect repairing agent, the pure ZIF-67 film is directly repaired in situ in one step to synthesize a defect-free ZIF-67 film, which is simple and fast, does not require high temperature and high pressure treatment, and does not need to introduce toxic organic molecules. The defects on the membrane surface can be repaired. This greatly reduces the production cost, improves the production efficiency, and provides a new idea for repairing the defects on the membrane surface.

Description

technical field [0001] The invention belongs to the field of preparation technology of dense inorganic membrane and gas separation technology, and in particular relates to a method for in situ repairing ZIF-67 film defects and the prepared film. Background technique [0002] As a new type of separation technology, membrane separation is considered to have good application prospects due to its low energy consumption, high separation efficiency, and simple and quick operation. Metal-organic framework membranes have attracted more and more attention from scholars because they integrate inorganic metal ions and organic ligands, and have both organic and inorganic properties. Due to its good thermal stability and stable performance, ZIF series membranes are currently the most researched. [0003] Although ZIF series membranes can theoretically be used in gas storage, sensing, catalysis, and gas separation, the main bottleneck restricting their development is that it is difficult...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D9/04C23C28/00
Inventor 王海辉侯倩倩周胜魏嫣莹
Owner SOUTH CHINA UNIV OF TECH
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