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Thin film composite film taking 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 problems such as difficulty in preparing large areas, inability to solve repeatability, cumbersome steps, etc., and achieve the effects of low cost, solving uneven distribution, and good repeatability

Active Publication Date: 2020-06-30
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 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 taking metal organic framework as functional layer, preparation method thereof and preparation method of metal organic framework
  • Thin film composite film taking metal organic framework as functional layer, preparation method thereof and preparation method of metal organic framework
  • Thin film composite film taking 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) 2-methylimidazole (0.692g, 8.4mmol) was dissolved in 10ml of polyethyleneimine (PEI) aqueous solution with a mass fraction of 5%, zinc nitrate hexahydrate (1.188g, 4.1mmol) was dissolved in 6ml of After mixing the two solutions in deionized water, the solution turned milky white, stirred at room temperature for 10 minutes, then added 35ml of absolute ethanol, and stirred for another 2 hours.

[0087] 2) Use a sprayer to spray the obtained solution on the polyacrylonitrile substrate with an area of ​​4.5cm*4.5cm, 10 times. The conditions for spraying are: the heating temperature of the heating plate where the substrate is located is 60°C, the flow rate is 0.2ml / min, and the needle is away from the substrate. 5cm, ambient temperature room temperature. Obtain a film (named ZIF-L film) with a layer of ZIF-L with uniform thickness on the surface, from figure 1 It can be found from the scanning electron microsco...

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) Use a sprayer to spray the obtained dispersion on the polyacrylonitrile substrate with an area of ​​4.5cm*4.5cm and spray it 25 times. 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 the recei...

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*4.5cm 30 times. The conditions used for spraying are: the heating temperature of the heating plate where the substrate is located is 70°C, and the flow rate is 0.15ml / min. The needle is 4 cm away from the substrate, and 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...

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Abstract

The invention provides a preparation method of a thin film composite film taking a metal organic framework as a functional layer, which comprises the following steps: 1) mixing a metal organic framework mixed solution containing a polyamine with an alcohol to obtain a dispersion solution; (2) spraying the dispersion liquid obtained in the step (1) on a base film by utilizing a spraying technology,so that a uniform metal organic framework layer is formed on the surface of the base film; and 3) spraying a polybasic acyl chloride solution on the surface of the metal organic framework layer prepared in the step 2) by using a spraying technology, and generating a polyamide layer by using an interfacial polymerization reaction to fix the metal organic framework, thereby obtaining the thin filmcomposite film. According to the invention, the spraying technology is applied to the construction of the metal organic framework film composite film; the problems that large-scale preparation of themetal organic framework film composite film is difficult and repeatability is poor are solved, the metal organic framework film composite film with a thin functional layer and excellent dye interception performance can be prepared, and the prepared MOF film composite film has a very high industrial application prospect.

Description

technical field [0001] The invention relates to the field of filter membranes, in particular to a 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 framework is a kind of porous material, which is self-assembled by the coordination bonds of metal ions and organic ligands. It has many outstanding advantages, such as high specific surface area, easy to flexibly adjust the main structure and pore diameter, etc. Due to their excellent properties, metal-organic frameworks (MOFs) have promising application prospects in a large number of 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 environmental protection and low energy consumption. At the same time, the performance of separation and the size of flux...

Claims

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Application Information

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Patent Type & Authority Applications(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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