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Method for preparing metal organic framework molecular sieve membrane by supercritical fluid technology

A metal-organic framework and supercritical fluid technology, applied in the field of membrane separation, achieves the effect of industrial route green environmental protection, broad application prospects, and excellent membrane separation performance

Active Publication Date: 2020-08-28
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using supercritical CO 2 As a green reaction medium, the MOF molecular sieve membrane with good separation performance is prepared on the commercial porous carrier modified by the metal precursor layer, which effectively solves the problem of both environmental protection and excellent separation performance in the current membrane preparation process. long-term constraints

Method used

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  • Method for preparing metal organic framework molecular sieve membrane by supercritical fluid technology
  • Method for preparing metal organic framework molecular sieve membrane by supercritical fluid technology
  • Method for preparing metal organic framework molecular sieve membrane by supercritical fluid technology

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Porous Supports Modified with Metal Oxide Layers: Sol-Gel Deposition

[0054] (1) Disperse and dissolve the metal salt in an organic solvent and stir to form a homogeneous solution, then add the alcohol amine aging metal salt solution to obtain a stable metal-based sol.

[0055] (2) Coating the metal-based sol on a clean porous alumina carrier (spin-coating / dip-coating for flat-plate / tubular supports, respectively, repeated coating 2-3 times), followed by calcination heat treatment to remove Solvent, the dense porous carrier modified by the metal oxide layer can be obtained.

[0056] (3) The sol-gel method deposition metal oxide layer modification steps involved in this embodiment 1 are all mature preparation processes, which do not belong to the protection scope of the present invention.

[0057] Prepare a uniform and dense zinc oxide modification layer on a flat plate porous alumina carrier by the above method, XRD ( figure 1 ) and SEM( figure 2 ) showed that a un...

Embodiment 2

[0061] Preparation of ZIF-8 Membrane by Supercritical Fluid Technology

[0062] 1. the zinc oxide (ZnO) layer prepared in embodiment 1 is modified the plate type porous alumina carrier support layer and is placed on the semi-permeable microreactor cavity in the supercritical kettle, and the 200mg solid state 2- Methylimidazole (2-mIm) ligand powder is placed below the cavity of the microreactor. Then gaseous CO 2 Enter the supercritical tank through the pre-compressor under high pressure, CO 2 The pressure is gradually increased to 10MPa, and the temperature is increased to 95°C, at this time the gaseous CO 2 into supercritical CO 2 And diffuse from below the microreactor into its cavity.

[0063] 2. In the chamber, supercritical CO 2 The solvent gradually dissolves the 2-mIm solid powder below the cavity to form a uniform supercritical CO that fully dissolves the organic ligand 2 Homogeneous reaction system, and diffused to fill the entire microreactor cavity, supercrit...

Embodiment 3

[0067] Preparation of ZIF-8 Membrane by Supercritical Fluid Technology

[0068] The difference with Example 2 is: in step 1, CO 2 The pressure is gradually increased to 10MPa, the temperature is increased to 35 ° C, and the rest of the steps are the same as in Example 2.

[0069] XRD( Figure 6 ) and SEM ( Figure 7 ) demonstrated that the surface-modified ZnO layer on the porous support transformed into a dense ZIF-8 film.

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Abstract

The invention discloses a method for preparing a metal organic framework (MOF) molecular sieve membrane by a supercritical fluid technology. The method comprises the following steps: firstly, puttinga porous carrier (support matrix) modified with a compact metal precursor layer and a solid organic ligand powder into a reactor cavity in a supercritical kettle; under the action of a supercritical fluid (CO2), gradually dissolving the solid organic ligand in the cavity to form a homogeneous reaction system; and carrying out a coordination reaction on the homogeneous reaction system and the metalprecursor layer in an interface region to form a continuous MOF molecular sieve membrane layer having excellent gas separation performance. In addition, the method for preparing the molecular sieve membrane by the supercritical fluid technology realizes zero emission and green cyclic utilization of all chemical reagents. In conclusion, the MOF molecular sieve membrane is prepared by the supercritical fluid technology, and the environmental protection of a membrane preparation process and the excellent separation performance of the molecular sieve membrane can be considered at the same time, so that the molecular sieve membrane has a good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of membrane separation, and in particular relates to a method for preparing a MOF molecular sieve membrane for a supercritical fluid technology and its gas separation application. Background technique [0002] The chemical separation process is one of the important energy-consuming steps in the chemical industry. Traditional separation technologies such as rectification separation are complex to operate and consume a lot of energy, so it is urgent to develop new separation technologies. Membrane separation technology has attracted wide attention due to its advantages such as simple operation, high separation efficiency, and environmental protection. In recent years, polymer membranes have been widely used in a variety of gas-liquid separation systems, but their separation performance suffers from the "Trade-off" effect. The problem also limits its further large-scale application. Polymorphic molecular sie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/76B01D67/00B01D53/22
CPCB01D53/228B01D67/0006B01D71/76
Inventor 刘毅刘亮亮
Owner DALIAN UNIV OF TECH
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