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Method for preparing MOF (at) MOF hybrid membrane by using two-dimensional nanosheet membrane induced heteroepitaxial growth method

A heteroepitaxy, two-dimensional nanotechnology, applied in chemical instruments and methods, separation methods, membrane technology, etc., to achieve excellent molecular sieving performance, simple and efficient preparation method, and high selectivity

Active Publication Date: 2021-04-16
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the deficiencies of the existing technology, the present invention aims at the difficult problem of the preparation of high-performance polycrystalline hybrid MOF separation membranes. The present invention provides a method for preparing MOF@MOF hybrids using a two-dimensional nanosheet film-induced heteroepitaxial growth method. Membrane method, the method first introduces the ZnO nanoparticle active layer on the surface of the porous support by sol-gel method, and in situ self-transformation into two-dimensional ZnO in the synthesis solution of benzimidazole organic ligand without metal source 2 (bIm) 4 Nanosheet film layer; then the carrier with two-dimensional nanosheet film layer is placed in the ZIF-8, ZIF-67 or Zn / Co-ZIF synthesis solution, and the Zn 2 (bIm) 4 @ZIF-8, Zn 2 (bIm) 4 @ZIF-67 or Zn 2 (bIm) 4 @Zn / Co-ZIF hybrid film

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  • Method for preparing MOF (at) MOF hybrid membrane by using two-dimensional nanosheet membrane induced heteroepitaxial growth method
  • Method for preparing MOF (at) MOF hybrid membrane by using two-dimensional nanosheet membrane induced heteroepitaxial growth method
  • Method for preparing MOF (at) MOF hybrid membrane by using two-dimensional nanosheet membrane induced heteroepitaxial growth method

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Embodiment 1

[0023] A method for preparing a MOF@MOF hybrid film by using a two-dimensional nanosheet film-induced heteroepitaxial growth method;

[0024] Step (1): An alumina porous ceramic tube with an average pore diameter of 200 nm was selected as a carrier, ultrasonically cleaned with absolute ethanol for 30 min before use, and then dried in a vacuum oven at 80° C. for 1 h.

[0025] Step (2): Mix 8.2624g of zinc acetate and 50mL of ethylene glycol methyl ether, and stir in a water bath at 70°C for 30min, then slowly add 4.6mL of ethanolamine dropwise, and stir at room temperature for 24h to obtain a zinc sol, and then in the porous The zinc sol was pulled three times on the surface of the ceramic tube, dried in an oven at 100°C for 1 hour after each pull, and finally calcined in a muffle furnace at 400°C for 200 minutes to obtain a carrier with an active layer of ZnO nanoparticles.

[0026] Step (3): The carrier with the ZnO nanoparticle active layer obtained in step (2) is placed in ...

Embodiment 2

[0029] A method for preparing a MOF@MOF hybrid film by using a two-dimensional nanosheet film-induced heteroepitaxial growth method;

[0030] Step (1), step (2) and step (3) are the same as embodiment 1.

[0031] Step (4): with two-dimensional Zn obtained in step (3) 2 (bIm) 4 The carrier of the nanosheet film layer is placed in the ZIF-67 synthesis solution, and its molar ratio is specifically cobalt nitrate: dimethylimidazole: deionized water molar ratio of 1:75:6000. The synthesis temperature is 100°C, and the synthesis time is 12h. After the reaction, the ceramic tube carrier was taken out, and the surface of the membrane layer was gently washed with methanol, and then dried in a vacuum oven at 60°C for 12 hours to obtain Zn 2 (bIm) 4 @ZIF-67 hybrid membrane.

Embodiment 3

[0033] A method for preparing a MOF@MOF hybrid film by using a two-dimensional nanosheet film-induced heteroepitaxial growth method;

[0034] Step (1), step (2) and step (3) are the same as embodiment 1.

[0035] Step (4): with two-dimensional Zn obtained in step (3) 2 (bIm) 4 The carrier of the nanosheet film layer is placed in the Zn / Co-ZIF synthesis solution, and the molar ratio is specifically zinc nitrate: cobalt nitrate: dimethylimidazole: deionized water molar ratio is 0.5:0.5:75:6000. The synthesis temperature is 100°C, and the synthesis time is 12h. After the reaction, the ceramic tube carrier was taken out, and the surface of the membrane layer was gently washed with methanol, and then dried in a vacuum oven at 60°C for 12 hours to obtain Zn 2 (bIm) 4 @Zn / Co-ZIF hybrid film.

[0036] To the Zn prepared in the embodiment of the present invention 1 2 (bIm) 4 The @ZIF-8 hybrid membrane was tested for gas separation, and its H 2 / CO 2 、H 2 / N 2 、H 2 / CH 4 Th...

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Abstract

The invention belongs to the field of MOF membrane preparation, and discloses a method for preparing an MOF (at) MOF hybrid membrane by using a two-dimensional nanosheet membrane induced heteroepitaxial growth method. The method comprises the following steps: firstly, pulling and introducing a ZnO nanoparticle active layer on the surface of a porous carrier through a sol-gel method, and putting the carrier into an organic ligand synthetic liquid without a metal source to be self-converted into a two-dimensional Zn2 (bIm) 4 nanosheet type film layer; then, placing the carrier with the two-dimensional nanosheet type film layer in another MOF synthetic liquid, generating another MOF crystal through induction of a two-dimensional nanosheet base film and filling the space between sheet layers of the two-dimensional nanosheet, filling gaps between the sheet layers, and generating the continuous MOF (at) MOF hybrid film. The preparation method is simple and efficient, large-area film forming can be achieved, a new strategy for preparing the high-quality MOF (at) MOF hybrid film is developed, and the method has wide application prospects.

Description

technical field [0001] The invention belongs to the field of MOF membrane preparation, and the invention relates to a method for preparing MOF@MOF hybrid membranes by using a heterogeneous epitaxial growth method induced by two-dimensional nanosheet membranes. It provides a new way to prepare high-performance polycrystalline hybrid MOF membranes. Background technique [0002] The membrane separation process has the advantages of low energy consumption, simple equipment, environmental friendliness, and easy cross-application with other technologies, so it is widely used in chemical, electronic, food and other industrial fields. It is considered to be one of the most promising emerging technology industries. However, the separation performance of traditional membrane materials is often limited by the interaction between permeability and selectivity (Robertson's upper limit), which hinders the further research progress of membrane separation. difficulties and key points. [0...

Claims

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Application Information

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IPC IPC(8): B01D71/06B01D71/02B01D69/12B01D53/22
Inventor 张雄福马畅畅刘海鸥
Owner DALIAN UNIV OF TECH
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