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Preparation method for ZIFs membrane containing zinc adopting sandwich structure and supported by high temperature resistant zinc oxide nanorod

A technology of zinc oxide nanorods and organic frameworks, applied in chemical instruments and methods, membrane technology, semipermeable membrane separation, etc. Weak carrier force and other issues, to achieve good change elasticity and operation and high temperature stability, high stability, mild condition effect

Active Publication Date: 2013-11-27
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation methods can be divided into three categories: (1) In situ growth method: [Aguado, et al., New J.Chem., 2011,35:41-44.] directly put the carrier into the film-forming solution by hydrothermal or Metal-organic framework membranes are obtained by solvothermal for a certain period of time. Due to the difference in properties between metal-organic materials and the surface of the support, this method is difficult to prepare dense metal-organic framework membranes; (2) Support surface modification method: using aminopropylsilane coupling agent [Aisheng Huang, et al., J.Am.Chem.Soc., 2010,132:15562-15564] handle the carrier and rely on weak coordination to connect the film layer. In this method, the force between the film layer and the carrier is relatively weak; (3) Seed secondary growth method: use viscous polymer materials (polyethyleneimine, PEI) to connect nano-scale metal-organic framework materials on the surface of the carrier to obtain a seed layer, and obtain a dense film layer through secondary growth in the synthetic solution , this method eliminates the performance difference between metal-organic and inorganic carrier surfaces, and is a typical preparation method in current reports, but this method needs to prepare nano-scale seeds with uniform size first, and the synthesis process has many steps, which increases the preparation process
At present, the preparation of metal-organic framework membranes is still immature, and the carriers used for the preparation of metal-organic framework membranes are mostly flakes.

Method used

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  • Preparation method for ZIFs membrane containing zinc adopting sandwich structure and supported by high temperature resistant zinc oxide nanorod
  • Preparation method for ZIFs membrane containing zinc adopting sandwich structure and supported by high temperature resistant zinc oxide nanorod
  • Preparation method for ZIFs membrane containing zinc adopting sandwich structure and supported by high temperature resistant zinc oxide nanorod

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Experimental program
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Embodiment 1

[0027] (1) The porous carrier is α-Al with an average pore diameter of about 0.1 μm 2 o 3 ceramic carrier tube. Before the synthesis, the carrier is first subjected to ultrasonic vibration treatment, then the carrier is cleaned with deionized water, and dried for later use.

[0028] (2) A certain amount of zinc acetate was dissolved in ethylene glycol methyl ether solvent and ethanolamine was used as a stabilizer to obtain a sol with a mass fraction of zinc of 12 wt%. Then the porous carrier was dipped and pulled to coat the pre-configured zinc sol, dried at 100°C for 2 hours, and repeated twice. Roast at 400°C for 2h, and set the heating rate at 1°C / min;

[0029] (3) Put the carrier tube with nano-zinc oxide seed crystals into a hydrothermal kettle containing a synthetic solution of 0.1M zinc nitrate hexahydrate and 0.1M hexamethylenetetramine and react at 100°C for 3h to obtain rod-shaped oxide Alumina ceramic tube with zinc rods.

[0030] (4) Put the porous ceramic tub...

Embodiment 2

[0033] (1)~(3) are the same as Example 1;

[0034] (4) Put the porous ceramic tube with rod-shaped zinc oxide into the prepared 0.5M 2-methylimidazole ethanol activation solution for activation at 50°C for 10 minutes, take it out and dry it in the air;

[0035] (5) After activation, the porous ceramic tube of rod-shaped zinc oxide is placed in a ratio of HCOONa:ZnCl 2 :2-meIM:MeOH=1.5:1.0:1.5:900 film synthesis solution, grow film at 100℃ for 5h. Cool the reaction kettle to room temperature naturally, take out the ceramic tube, slowly rinse the surface of the film layer to remove the crystals attached to the surface layer, dry it naturally and place it in a desiccator for testing.

Embodiment 3

[0037] (1)~(3) are the same as Example 1;

[0038] (4) Put the porous ceramic tube with rod-shaped zinc oxide into the prepared 0.5M 2-methylimidazole water activation solution for activation at 50°C for 0.5h, take it out and dry it in the air;

[0039] (5) After activation, the porous ceramic tube of rod-shaped zinc oxide is placed in a ratio of HCOONa:ZnCl 2:2-meIM:MeOH=1.5:1.0:1.5:900 film synthesis solution, grow film at 100℃ for 2h. Cool the reaction kettle to room temperature naturally, take out the ceramic tube, slowly rinse the surface of the film layer to remove the crystals attached to the surface layer, dry it naturally and place it in a desiccator for testing.

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Abstract

The invention discloses a preparation method for a novel ZIFs membrane containing zinc adopting sandwich structure and supported by a high temperature resistant zinc oxide nanorod. According to the invention, by introducing a layer of zinc oxide nanorod on a porous carrier as a bridge to connect the carrier and the ZIFs membrane to construct to form the sandwich structural membrane supported by the zinc oxide nanorod. The zinc oxide nanorod has the following functions: 1, modifying the carrier surface to facilitate the uniform growth of the ZIFs membrane; 2, acting as homogeneous phase induction nucleation growing point of the continuous growth of the ZIFs membrane to guarantee the complete formation of the membrane with high sieving property; acting as bridging liking effect between the carrier and the membrane layer to solve the combination problem between the membrane and the carrier and guarantee high stability of the membrane. Compared with a traditional preparation method of a ZIFs membrane, the membrane prepared by the invention not only has high separating property, high temperature resistance, but also has simple process, good repeatability, convenience in amplification of large-scale preparation, and wide application prospect.

Description

technical field [0001] The invention provides a method for preparing a zinc-containing metal-organic framework membrane with a sandwich structure supported by high-temperature-resistant zinc oxide nanorods, which is applied to gas separation at high temperatures. The main purpose is to provide a high-performance metal-organic framework membrane with a new structure, and to solve the problem of the binding force between the membrane and the carrier. technical background [0002] Metal-organic framework (MOFs) materials are a very hot field of research in recent years. Due to their large specific surface area, good hydrothermal stability and some special chemical properties, they can be used in gas storage and separation, catalysts, drug slow release, sensors etc. Especially in today's society, energy and carbon emissions are increasingly becoming the focus of the whole society. MOFs will be an important material for human beings to solve the above problems, and their applica...

Claims

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Application Information

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IPC IPC(8): B01D71/06B01D67/00B01D69/10
Inventor 张雄福李绍辉刘亚光孔令寅刘海鸥邱介山
Owner DALIAN UNIV OF TECH
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