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Simple solvothermal growth method for preparing oriented growing metal organic skeleton nanometer slice film

A metal-organic framework and orientation growth technology, applied in the field of metal-organic framework sheet membranes, can solve the problems of complexity, difficulty, and difficulty in preparing nanosheet membranes, and achieve the effects of less pollution, environmental friendliness, good amplification and application prospects.

Active Publication Date: 2016-07-27
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the complex and difficult problem of preparing metal-organic framework nano-sheet membranes, the present invention proposes a new method for preparing metal-organic framework nano-sheet membranes by a simple solvothermal growth method. The positioning active points of the skeleton nanosheet membrane, that is, first grow a layer of zinc oxide (ZnO) on the surface of the carrier as the positioning active points through hydrothermal synthesis to obtain a carrier with a ZnO nanolayer; then place the carrier on the metal-organic framework The nanosheet film synthesis solution is synthesized by a solvothermal system, and the continuous and uniformly oriented MOFs nanosheet film is formed after finely regulated growth
This preparation method solves the difficult and complicated problem of the preparation of metal-organic framework nano-sheet membranes. It is simple and convenient and can be formed on a large-area carrier, and has good scale-up and application prospects.

Method used

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  • Simple solvothermal growth method for preparing oriented growing metal organic skeleton nanometer slice film
  • Simple solvothermal growth method for preparing oriented growing metal organic skeleton nanometer slice film
  • Simple solvothermal growth method for preparing oriented growing metal organic skeleton nanometer slice film

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Choose an alumina porous ceramic carrier tube with an average pore diameter of about 0.2 μm, and clean it before use.

[0028] (2) 8.2624g of zinc acetate was dissolved in 50mL of ethylene glycol methyl ether solvent and 4.6mL of ethanolamine was used as a stabilizer to prepare a zinc oxide sol solution containing 30% zinc by mass fraction. Then, a zinc sol layer was formed on the alumina ceramic carrier tube in (1) by pulling coating, and dried at 100° C. for 1 h, and repeated 3 times. After drying, it was baked in a muffle furnace at a temperature of 500° C. for 4 hours according to a programmed temperature to obtain a porous carrier with a zinc oxide coating.

[0029] (3) the ceramic carrier with zinc oxide particle layer in (2), put into containing bIm quality and be 1.15g molar ratio be bIm:NH 3 ·H 2 O:PhMe:CH 3 OH=1:3:20:60 in the synthesis solution, react at 60°C for 5 minutes, take it out and wash it with methanol, then put it into the synthesis solution ...

Embodiment 2

[0031] (1) and (2) are the same as example 1.

[0032] (3) have the ceramic carrier of zinc oxide particle layer, put into containing bIm quality and be 1.15g mol ratio be bIm:NH 3 ·H 2 O:PhMe:CH 3In the synthesis solution of OH=2:1:40:60, react at 30°C for 10 minutes, take it out and wash it carefully with methanol, then put it into the synthesis solution again for 10 minutes, and repeat this operation 5 times. Finally, the ceramic tube was taken out, the surface of the film layer was slowly rinsed with methanol, and dried naturally to obtain a nanosheet film with horizontal orientation growth.

Embodiment 3

[0034] (1) and (2) are the same as example 1.

[0035] (3) Suspend the alumina ceramic tube with zinc oxide particles in an 80mL aqueous synthesis kettle containing 2.3798g of zinc nitrate and 1.1216g of hexamethylenetetramine, and react at 100°C for 5h to obtain zinc oxide nano-array rods. Ceramic tube.

[0036] (4) will have the ceramic carrier of zinc oxide nano-array rod, insert the quality that contains bIm and be 1.15g molar ratio be bIm:NH 3 ·H 2 O:PhMe:CH 3 In the synthesis solution of OH=1:1:40:60, the solvothermal growth reaction was carried out at 120°C for 24 hours, and the film tube was taken out and slowly rinsed with methanol on the surface of the film layer, and then dried naturally to obtain the nanosheet film grown in the vertical direction.

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Abstract

The invention relates to a simple solvothermal growth method for preparing an oriented growing metal organic skeleton nanometer slice film. The method comprises the following steps: introducing a positioning active point for the oriented growth of the metal organic skeleton nanometer slice film on the surface of a carrier, namely, growing a layer of nanoscale zinc oxide as the positioning active point for metal central ion coordinate on the carrier surface through hydro-thermal synthesis, thereby acquiring a carrier with ZnO nanometer layer positioning active point; putting the carrier into a synthesis solution of the metal organic skeleton nanometer slice film and compounding through a solvothermal system; and controlling growth, thereby forming the continuous and uniform horizontal or vertical oriented metal organic skeleton nanometer slice film. The preparation method solves the problem of difficulty and complexity of preparation of a metal organic skeleton nanometer slice film and has the advantages of simpleness, convenience, capability of forming film on large-area carriers and excellent amplifying and application prospect.

Description

technical field [0001] The invention provides a simple solvothermal growth method to directly prepare an orientationally grown metal-organic framework sheet membrane, and solves the difficult problem of forming a continuous metal-organic framework sheet membrane on the surface of a ceramic tube carrier. It opens up a new way for the preparation of high-performance metal-organic framework sheet membranes. Background technique [0002] In recent years, the research on metal-organic frameworks (MOFs) has been a hot spot of attention. This type of material has a similar topology to zeolite molecular sieves. It is an inorganic-organic hybrid porous material, because the pore size can be adjusted by organic ligands and inorganic The metal center can be rationally controlled, and the surface can also be treated with a series of functionalization, so MOFs materials attract people to prepare them into membranes for gas and liquid separation applications. The number of research repor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D69/10B01D71/76B01D67/00B01D69/04B01D69/06C08G83/00
CPCB01D67/0079B01D69/04B01D69/06B01D69/10B01D69/105B01D71/76C08G83/008
Inventor 张雄福李雨佳刘海鸥邱介山
Owner DALIAN UNIV OF TECH
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