Method for preparing MOF nanofiltration membrane by adopting thermal annealing post-synthesis technology

A thermal annealing and nanofiltration membrane technology, applied in the field of membrane separation, can solve problems such as the stability limitation of separation membranes, and achieve the effect of changing the type and size of pore channels, simplifying the process, and increasing flux

Active Publication Date: 2020-09-18
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The swelling problem of the nanofiltration membrane in the solvent for a long time is the key factor affecting its stability. At present, there are two main methods to solve the problem of swelling resistance of the separation membrane: one is to use an inorganic membrane with good solvent resistance itself; two. It is a modified organic polymer material, such as increasing its cross-linking degree, etc., but the stability of the final separation membrane is still limited by the organic polymer itself

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The ceramic substrate used is a commercial tubular ceramic single-hole outer membrane with an outer diameter of 13mm, an inner diameter of 10mm, and a membrane area of ​​0.001m 2 , the selected precursor metal ion is cobalt nitrate, the organic ligand is 2-methylimidazole, the gelling agent is ethanolamine, the nucleating agent is cetyltrimethylammonium bromide, and the selected solvent is ethanol.

[0030] Preparation method for synthesizing modified MOF composite membrane after thermal annealing:

[0031] (1) Perform ultrasonic pretreatment on the commercial porous tubular ceramic substrate, first soak the substrate in deionized water, and then ultrasonically oscillate for 1-10 minutes to remove impurities on the surface and inside of the substrate;

[0032] (2) Dry the substrate after ultrasonic oscillation with deionized water at 60°C before use;

[0033] (3) Dissolve the MOF-forming precursor, 4.35g of cobalt nitrate and 0.9g of ethanolamine in an ethanol solvent ...

Embodiment 2

[0041] The ceramic substrate used is a commercial tubular ceramic single-hole outer membrane with an outer diameter of 13mm, an inner diameter of 10mm, and a membrane area of ​​0.001m 2 , the selected precursor metal ion is cobalt nitrate, the organic ligand is 2-methylimidazole, the gelling agent is ethanolamine, the nucleating agent is cetyltrimethylammonium bromide, and the selected solvent is ethanol.

[0042] Preparation method for synthesizing modified MOF composite membrane after thermal annealing:

[0043] (1) Perform ultrasonic pretreatment on the commercial porous tubular ceramic substrate, first soak the substrate in deionized water, and then ultrasonically oscillate for 1-10 minutes to remove impurities on the surface and inside of the substrate;

[0044] (2) Dry the substrate after ultrasonic oscillation with deionized water at 60°C before use;

[0045] (3) Dissolve the MOF precursor, 4.35g of cobalt nitrate metal ion and 0.9g of ethanolamine in 100mL of ethanol ...

Embodiment 3

[0053] The ceramic substrate used is a commercial tubular ceramic single-hole outer membrane with an outer diameter of 13mm, an inner diameter of 10mm, and a membrane area of ​​0.001m 2 , the selected precursor metal ion is cobalt nitrate, the organic ligand is 2-methylimidazole, the gelling agent is ethanolamine, the nucleating agent is cetyltrimethylammonium bromide, and the selected solvent is ethanol.

[0054] Preparation method for synthesizing modified MOF composite membrane after thermal annealing:

[0055] (1) Perform ultrasonic pretreatment on the commercial porous tubular ceramic substrate, first soak the substrate in deionized water, and then ultrasonically oscillate for 1-10 minutes to remove impurities on the surface and inside of the substrate;

[0056] (2) Dry the substrate after ultrasonic oscillation with deionized water at 60°C before use;

[0057] (3) Dissolve the MOF precursor, 4.35g of cobalt nitrate metal ion and 0.9g of ethanolamine in 100mL of ethanol ...

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Abstract

The invention provides a method for preparing an MOF nanofiltration membrane by adopting a synthesis technology after thermal annealing, and belongs to the field of membrane separation, wherein the method comprises the following steps: carrying out ultrasonic pretreatment on a porous ceramic substrate, activating and cleaning the surface of the ceramic substrate; firstly, coating the surface of the ceramic substrate with metal gel, then placing the ceramic substrate in a solution containing organic ligands, and enabling MOF nanoparticles to grow on the ceramic substrate in situ to form a continuous defect-free MOF separation layer; carrying out high-temperature post-synthesis modification on the synthesized MOF composite membrane, and activating the internal microstructure of the MOF particles and regulating and controlling the thickness and morphology of an MOF separation layer by regulating and controlling the annealing temperature, the annealing time, the heating rate, the cooling rate and the like. The MOF separation membrane prepared by the method disclosed by the invention is good in binding force with a substrate, and the mass transfer rate in the separation process can be effectively improved, so that the flux of the separation membrane is improved under the condition of not sacrificing the rejection rate.

Description

technical field [0001] The invention relates to a method for preparing MOF nanofiltration membranes by adopting thermal annealing post-synthesis technology, which is used for nanofiltration separation and belongs to the field of membrane separation. Background technique [0002] Nanofiltration technology is a separation process between reverse osmosis and ultrafiltration, with high selectivity, low energy consumption and simple operation. Due to its many advantages, it has been widely used in petrochemical, pharmaceutical and food fields. The swelling problem of the nanofiltration membrane in the solvent for a long time is the key factor affecting its stability. At present, there are two main methods to solve the problem of swelling resistance of the separation membrane: one is to use an inorganic membrane with good solvent resistance; It is a modified organic polymer material, such as increasing its cross-linking degree, etc., but the stability of the final separation membr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D69/12B01D69/02B01D61/00
CPCB01D67/0083B01D69/02B01D69/12B01D61/027
Inventor 王乃鑫李晓婷孙皓王湘琼李杰安全福
Owner BEIJING UNIV OF TECH
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