Preparation method for synthesizing ZIF-67 membrane through in-hole membrane formation

A ZIF-67, film-forming technology, applied in separation methods, chemical instruments and methods, membranes, etc., can solve the problems of high process difficulty, swelling, poor stability, low strength, etc., to reduce environmental pollution and simple preparation process. , high repeatability

Inactive Publication Date: 2021-06-25
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, membrane materials are mainly divided into two categories: inorganic membranes and organic membranes. Organic polymer membranes are corrosion-resistant and easy to form and process, but have the disadvantages of swelling and poor stability. Due to their excellent thermal and chemical stability, inorganic membranes Compared with the traditional zeolite membrane, the ZIFs series membrane not only has all the advantages of zeolite, but also has adjustable pore size, and the surface is easy to chemical Modified features, is a promising membrane material
[0004] At present, the synthesis of membranes mainly includes in-situ growth method, seed crystal induction method, homologous...

Method used

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  • Preparation method for synthesizing ZIF-67 membrane through in-hole membrane formation
  • Preparation method for synthesizing ZIF-67 membrane through in-hole membrane formation
  • Preparation method for synthesizing ZIF-67 membrane through in-hole membrane formation

Examples

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Effect test

Embodiment 1

[0040] (1) Pretreatment α-Al 2 o 3Carrier tube: the outer diameter of the tube is 12mm, the inner diameter of the tube is 8mm, the average pore diameter is 2-3μm, and the porosity is about 30-40%; the outer surface of the carrier tube is polished with 800 mesh and 1500 mesh sandpaper; it is removed by ultrasonic vibration with deionized water The remaining sand particles on the carrier tube are repeated several times until the water used for washing the tube is no longer turbid, then ultrasonically shake with acid and alkali in order to remove the residue in the carrier pores, and wash with deionized water until neutral; finally The tube was dried in an oven, then calcined in a muffle furnace at 550°C for 6 hours, and both ends were sealed for later use;

[0041] (2) Add 5g of cobalt acetate and 30mL of ethylene glycol methyl ether into a 100mL beaker, stir in a water bath at 75°C for 60min, then add 2ml of 2-aminoethanol, and stir at room temperature for 12h to obtain a prec...

Embodiment 2

[0046] (1) Pretreatment α-Al 2 o 3 Carrier tube: the outer diameter of the tube is 12mm, the inner diameter of the tube is 8mm, the average pore diameter is 2-3μm, and the porosity is about 30-40%; the outer surface of the carrier tube is polished with 800 mesh and 1500 mesh sandpaper; it is removed by ultrasonic vibration with deionized water The remaining sand particles on the carrier tube are repeated several times until the water used for washing the tube is no longer turbid, then ultrasonically shake with acid and alkali in order to remove the residue in the carrier pores, and wash with deionized water until neutral; finally The tube was dried in an oven, then calcined in a muffle furnace at 550°C for 6 hours, and both ends were sealed for later use;

[0047] (2) Add 5g of cobalt nitrate hexahydrate and 30mL of ethylene glycol methyl ether into a 100mL beaker, stir in a water bath at 75°C for 60min, then add 2ml of 2-aminoethanol, and stir at room temperature for 12h to ...

Embodiment 3

[0052] The gas-phase filled synthetic ZIF-67 membrane prepared in Example 1 was tested for single-component gas and pressure, and the test results are shown in the figure below. After testing, H 2 The permeate flux range is 2.50×10 -7 mole m -2 ·s -1 pa -1 , H 2 / CH 4, The separation factor is 15, which is far greater than Knudsen diffusion, which proves the feasibility of this method and has a certain separation ability for gases; when the pressure is increased, H 2 / CH 4 The separation factor remained basically stable, indicating strong applicability.

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Abstract

The invention belongs to the technical field of separation materials, and provides a preparation method for synthesizing a ZIF-67 membrane through in-hole membrane formation, which specifically comprises the following steps: introducing a precursor solution of cobalt into a porous carrier pore channel, suspending the carrier in a kettle containing a certain amount of ligand solution, forming steam from the solution in the kettle under a heating condition, and forming a membrane at a phase interface by the steam formed by the solution in the kettle and the precursor solution in the pore channel. Although the membrane is divided into countless small membranes by each hole wall, each membrane is formed in a small space, is relatively complete and thin, and has no gap with the hole wall, a plurality of complete membranes and the hole wall form a large complete membrane together, and the membrane is not a large membrane, so that the membrane can be thin and has good stability, and the purpose of separation is achieved. The method has the advantages of high repeatability, effective solvent saving and certain separation capability.

Description

technical field [0001] The invention belongs to the technical field of separation materials, and relates to the preparation and application of a metal organic framework, in particular to a preparation and application method of zeolite-like imidazole framework compounds. Background technique [0002] my country is the largest coke production, consumption and exporter in the world. A large amount of coke oven gas will be produced in the coke production process. The main components of coke oven gas are methane, hydrogen and a small amount of nitrogen. If the coke oven gas can be fully Utilization will be a considerable economic income. Therefore, it is particularly important to realize the efficient separation of hydrogen and methane. [0003] Membrane separation is an advanced separation technology developed in recent years. It is known as one of the most potential high-end separation technologies. It has the advantages of environmental friendliness, low energy consumption, sma...

Claims

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Application Information

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IPC IPC(8): B01D67/00B01D71/06B01D69/02B01D53/22
CPCB01D67/0006B01D71/06B01D69/02B01D53/228B01D2325/24
Inventor 鲁金明尚鸿飞杨建华刘毅张艳王金渠
Owner DALIAN UNIV OF TECH
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