Method of preparing high-orientation two-dimensional metal-organic frameworks nanosheet-type film through induced growth of zinc oxide in limited range of graphene oxide

A metal-organic framework and nanosheet technology, applied in chemical instruments and methods, separation methods, membrane technology, etc., can solve the problems of complex preparation of 2DMOFs nanosheet membranes, difficulties and difficulties in the preparation of nanosheet membranes, etc., and achieve excellent gas Separation effect, good magnification and application prospects, high orientation effect

Active Publication Date: 2017-12-01
DALIAN UNIV OF TECH
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0005] The present invention aims at the complex and difficult problem of preparing 2D MOFs nanosheet membranes in the prior art, and proposes a new method for preparing highly oriented two-dimensional MOFs sheet membranes by graphite oxide-confined zinc oxide (ZnO) induced growth method
This preparation method solves the difficulty and complexity of the preparation of metal-organic framework nanosheet membranes, and 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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  • Method of preparing high-orientation two-dimensional metal-organic frameworks nanosheet-type film through induced growth of zinc oxide in limited range of graphene oxide
  • Method of preparing high-orientation two-dimensional metal-organic frameworks nanosheet-type film through induced growth of zinc oxide in limited range of graphene oxide
  • Method of preparing high-orientation two-dimensional metal-organic frameworks nanosheet-type film through induced growth of zinc oxide in limited range of graphene oxide

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Experimental program
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Effect test

Embodiment 1

[0030] (1) The carrier is an alumina ceramic tube carrier with an average pore diameter of about 0.1-2 μm. Before synthesis, use deionized water and ethanol to ultrasonically wash several times to remove surface particles and stains, and dry them for later use.

[0031](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 form a ZnO sol solution with a mass fraction of zinc of 30%. Then, a zinc sol layer was formed on the alumina ceramic carrier tube in step (1) by pulling coating, and dried at 100° C. for 1 hour, and repeated 3 times. After drying, it was baked in a muffle furnace at a programmed temperature of 500° C. for 4 hours to obtain a porous carrier with a ZnO coating.

[0032] (3) Dissolve 0.2g of graphite oxide powder in 126mL of anhydrous methanol, and sonicate for 2h. Put the graphite oxide methanol solution into a centrifuge and centrifuge at 7000rpm for 30min, remove the ...

Embodiment 2

[0035] (1) and (2) are the same as embodiment 1 step (1) and step (2).

[0036] (3) Suspend the alumina ceramic tube with ZnO particles in an 80mL aqueous synthesis kettle containing 2.3798g zinc nitrate hexahydrate and 1.1216g hexamethylenetetramine, and react at 100°C for 5h to obtain ZnO nanoarray rods Ceramic tube.

[0037] (4) With embodiment 1 step (3).

[0038] (5) The ceramic carrier with ZnO nano-array rods and graphene oxide film is placed in a 1.15g molar ratio containing 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 12 hours, the film tube was taken out and the surface of the film layer was slowly rinsed with methanol, and then dried naturally to obtain a nanosheet film with horizontal orientation growth.

Embodiment 3

[0040] (1) With embodiment 1 step (1).

[0041] (2) 4.6322g of zinc acetate was dissolved in 50mL of ethylene glycol methyl ether solvent and 2.3mL of ethanolamine was used as a stabilizer to prepare a ZnO sol solution with a mass fraction of zinc of 15%. Then, the zinc sol layer was formed on the alumina ceramic carrier tube in step (1) by pulling once, and dried at 100° C. for 1 hour. After drying, it was baked in a muffle furnace at a programmed temperature of 500° C. for 4 hours to obtain a porous carrier with a ZnO coating.

[0042] (3) Dissolve 0.1 g of graphite oxide powder in 60 mL of anhydrous methanol, stir overnight, and sonicate for 2 h. Put the methanol solution of graphite oxide in a centrifuge and centrifuge at 7000rpm for 30min, remove the bottom dregs and take the supernatant, then add 60ml of anhydrous methanol, ultrasonicate for 2h, put it in the centrifuge and centrifuge at 10000rpm for 30min, remove the bottom dregs and take the supernatant. Then, pull f...

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Abstract

The invention provides a method of preparing a high-orientation two-dimensional metal-organic frameworks nanosheet-type film through induced growth of zinc oxide in a limited range of graphene oxide. According to the method, a locating active site of the MOFs (metal-organic frameworks) nanosheet-type film is introduced onto the surface of a carrier, in other words, a layer of nanoscale ZnO is grown on the surface of the carrier according to a sol-gel method to serve as the locating active site, and accordingly, the carrier with a ZnO nanolayer is obtained; a thin graphene oxide film is introduced onto the surface of the carrier through pulling to play a role in range limiting and inducing for growth of the nanosheet-type film; the carrier is put in MOFs nanosheet film compounding liquid for solvent thermal system compounding, the continuously-uniform high-orientation MOFs nanosheet-type film is formed through precisely regulated growth, and excellent gas separation effect and high stability and repeatability of the film are displayed. The method has the advantages that the problem that existing metal-organic frameworks nanosheet-type films are difficult and complex to prepare is solved, simplicity, convenience and film formation on large-area carriers are achieved, and the method has good amplification and application prospect.

Description

technical field [0001] The invention provides a graphene oxide-confined zinc oxide-induced growth to prepare a highly oriented two-dimensional metal-organic framework sheet film, which solves the problem of forming a continuous high-orientation two-dimensional metal-organic framework film on the surface of a porous carrier. It opens up a new way for the preparation of high-performance metal-organic framework sheet separation membranes. Background technique [0002] With the rapid development of two-dimensional (2D) scale graphene research, a series of 2D nanosheet materials such as zeolite molecular sieves, graphite oxide, transition metal sulfides, and boron nitride have also attracted more and more attention. These materials have a two-dimensional planar structure, large specific surface area, and other unique physical and chemical properties, and have a wide range of applications in the fields of catalysis, sensing, energy storage, and separation, which attract people to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D71/06B01D69/02B01D67/00B01D53/22
CPCB01D53/228B01D67/0079B01D69/02B01D71/024B01D71/06
Inventor 张雄福李雨佳刘海鸥
Owner DALIAN UNIV OF TECH
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