Thin film composite film with metal-organic framework as functional layer, preparation method thereof, and preparation method of metal-organic framework

A metal-organic framework and composite membrane technology, applied in the field of filtration membranes, can solve the problems of difficulty in preparing large areas, high costs, cumbersome steps, etc., and achieve high industrial application prospects, easy large-scale preparation, and good repeatability.

Active Publication Date: 2022-01-11
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has great limitations, such as poor repeatability and difficulty in preparing large-area non-negligible defects, and it is generally very thick, perhaps to a dozen microns
Other methods such as secondary growth and backdiffusion can produce a thin and dense MOF layer, but they still cannot solve the problem of reproducibility
Although there are many cutting-edge methods such as fast current-driven method and chemical vapor deposition method that can prepare MOF thin layers with good repeatability, their high cost, cumbersome steps and requirements for instruments limit their industrial application. sex

Method used

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  • Thin film composite film with metal-organic framework as functional layer, preparation method thereof, and preparation method of metal-organic framework
  • Thin film composite film with metal-organic framework as functional layer, preparation method thereof, and preparation method of metal-organic framework
  • Thin film composite film with metal-organic framework as functional layer, preparation method thereof, and preparation method of metal-organic framework

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] Preparation of ZIF-L thin film composite membrane:

[0086] 1) Dissolve 2-methylimidazole (0.692g, 8.4mmol) in 10ml of a 5% polyethyleneimine (PEI) aqueous solution, and dissolve zinc nitrate hexahydrate (1.188g, 4.1mmol) in 6ml of After mixing the two solutions in ionized water, the solution turned milky white, stirred at room temperature for 10 min, then added 35 ml of absolute ethanol, and stirred for another 2 h.

[0087] 2) The obtained solution was sprayed on the polyacrylonitrile substrate with an area of ​​4.5cm*4.5cm and 10 times using a spraying machine, and the spraying conditions were: the heating temperature of the heating plate where the substrate was located was 60°C, the flow rate was 0.2ml / min, and the needle was separated from the substrate. 5cm, ambient temperature room temperature. A film with a uniform thickness of ZIF-L on the surface (named as ZIF-L film) was obtained from figure 1 The scanning electron microscope image of the ZIF-L film shows t...

Embodiment 2

[0097] Similar to the method of Example 1, the metal organic framework used is UIO-66-NH 2 .

[0098] 1) 25mg of UIO-66-NH 2 After being added to 5 ml of 1% diethylenetriamine aqueous solution by mass fraction to obtain a mixed liquid, 30 ml of methanol was added to obtain a dispersion liquid.

[0099] 2) Spray the obtained dispersion on the polyacrylonitrile substrate with a spraying area of ​​4.5cm*4.5cm for 25 times using a spraying machine. The conditions used for spraying are: the heating temperature of the heating plate where the substrate is located is 50°C, and the flow rate is 0.2ml / min , the needle is 6cm away from the substrate, and the ambient temperature is room temperature. Get a surface with a layer of UIO-66-NH 2 The film (named UIO-66-NH 2 film), from Figure 10 The SEM image can be found that UIO-66-NH 2 There are a lot of particles on the surface of the membrane, which is granular UIO-66-NH 2 .

[0100] 3) Add UIO-66-NH 2 The membrane is glued to th...

Embodiment 3

[0103] Similar to the method of Example 1, the metal organic framework used is MIL-101-NH 2

[0104] 1) 45mg of MIL-101-NH 2 After being added to 5 ml of 1% triethylenetetramine solution by mass fraction to obtain a mixed solution, 40 ml of ethanol was added to obtain a dispersion.

[0105] 2) Use a sprayer to spray the obtained dispersion on the polyacrylonitrile substrate with an area of ​​4.5cm*4.5cm30 times. The conditions used for spraying are: the heating temperature of the heating plate where the substrate is located is 70°C, the flow rate is 0.15ml / min, the needle 4cm away from the substrate, the ambient temperature is room temperature. Get a sheet with a layer of MIL-101-NH on the surface 2 The film (named MIL-101-NH 2 film), from Figure 13 The SEM image can be found that MIL-101-NH 2 There are a lot of particles on the surface of the membrane, which is granular MIL-101-NH 2 .

[0106] 3) MIL-101-NH 2 The membrane is glued to the receiver roller of the elect...

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Abstract

The invention provides a method for preparing a thin film composite membrane with a metal-organic framework as a functional layer, comprising the following steps: 1) mixing a mixed solution of a metal-organic framework containing polyamines with alcohol to obtain a dispersion; 2) mixing step 1) The obtained dispersion is sprayed on the base film by spraying technology, so that the surface of the base film forms a uniform metal-organic framework layer; 3) spraying the polyacyl chloride solution on the surface of the metal-organic framework layer prepared in step 2) by spraying technology, The interfacial polymerization reaction is used to form a polyamide layer to fix the metal-organic framework to obtain a thin film composite membrane. The present invention applies the spraying technology to the construction of metal-organic framework thin film composite membranes, overcomes the problems of difficult scale-up and poor repeatability in the preparation of metal-organic framework thin-film composite membranes, and can prepare thinner functional layers and excellent dye retention performance The metal-organic framework thin film composite membrane prepared by MOF thin film composite membrane has a high industrial application prospect.

Description

technical field [0001] The invention relates to the field of filtration membranes, in particular to a thin film composite membrane with a metal-organic framework as a functional layer, a preparation method thereof, and a preparation method of the metal-organic framework. Background technique [0002] Metal-organic frameworks are porous materials composed of metal ions and organic ligands. Due to their excellent properties, metal-organic frameworks (MOFs) have promising applications in numerous fields, such as drug delivery, gas storage, catalysts, and sensors. [0003] In the field of material separation, membrane separation has their unique advantages, such as green environmental protection and low energy consumption. At the same time, the separation performance and flux size are the most concerned performance of membrane separation users. In order to improve the flux as much as possible while ensuring the material separation performance, the thin film composite membrane ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/56B01D69/12B01D67/00C08G83/00
CPCB01D71/56C08G83/008B01D69/125B01D67/0006
Inventor 徐铜文葛亮赵璋
Owner UNIV OF SCI & TECH OF CHINA
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