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MXene-based three-dimensional porous flexible self-supporting membrane, preparation method thereof and application of membrane in electrochemical adsorption of dyes

A three-dimensional porous, self-supporting membrane technology, applied in other chemical processes, separation methods, inorganic chemistry, etc., can solve the problems of small pore size, low specific surface area, and low adsorption performance of MXene nanofiltration membranes, and achieve easy recycling and improvement. Specific surface area, the effect of enhancing electrostatic effect

Active Publication Date: 2021-03-09
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the Chinese patent document CN109569317A provides a method for preparing MXene nanofiltration membranes, which uses ammonium hydrofluoride to etch a series of MAX materials to obtain the required MXene block materials, and decomposes large blocks of MXene by water vapor stripping into small nanosheets, and then use the solution intercalation method to embed tiny single-walled carbon nanotubes into the MXene nanosheets, and then prepare a new type of MXene nanofiltration membrane by means of vacuum filtration, but the MXene nanofiltration membrane pore size Relatively small, low specific surface area, relatively low adsorption performance
Chinese patent document CN110316719A provides a kind of MXene / nitrogen-doped carbon nanotube composite film and its preparation method. The preparation method includes the following steps: after mixing the MXene solution and the nitrogen-doped carbon nanotube solution, stirring for a period of time, and then, Suction filtration, natural air drying, to obtain MXene / nitrogen-doped carbon nanotube composite film, but the above composite film also has the disadvantages of relatively small pore size, low specific surface area, and relatively low adsorption performance

Method used

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  • MXene-based three-dimensional porous flexible self-supporting membrane, preparation method thereof and application of membrane in electrochemical adsorption of dyes
  • MXene-based three-dimensional porous flexible self-supporting membrane, preparation method thereof and application of membrane in electrochemical adsorption of dyes
  • MXene-based three-dimensional porous flexible self-supporting membrane, preparation method thereof and application of membrane in electrochemical adsorption of dyes

Examples

Experimental program
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Effect test

Embodiment 1

[0037] A kind of preparation method of MXene-based three-dimensional porous flexible self-supporting film, comprises steps as follows:

[0038] (1) Preparation of MXene nanosheet suspension

[0039] Add 2.5g LiF to 20mL HCl solution with a concentration of 6mol / L, stir evenly to obtain a mixed solution, and then add 2g Ti 3 AlC 2 Add it to the above mixed solution and react at 40°C for 48h; after the reaction, centrifuge and wash with deionized water until the pH of the supernatant is 6, vacuum dry the obtained solid at 60°C for 48h, then add deionized water for ultrasonic 90min, then centrifuged at 3500rpm for 60min, the resulting supernatant was Ti 3 C 2 T x MXene nanosheet suspension; known volume of Ti by suction filtration 3 C 2 T x After MXene nanosheet suspension and freeze-drying, the weight of the film was measured to calculate its concentration as 2mg / mL.

[0040] (2) Preparation of polystyrene microsphere suspension

[0041] Add 15mL of styrene and 1.5mL ...

Embodiment 2

[0050] A kind of preparation method of MXene-based three-dimensional porous flexible self-supporting membrane is as described in Example 1, the difference is: in step (3), the Ti concentration prepared by 10mL step (1) is 2mg / mL 3 C 2 T x MXene nanosheet suspension, the concentration of 1mL step (2) prepared is the polystyrene microsphere suspension of 5mg / mL, 1mL concentration is the single-walled carbon nanotube suspension of 1mg / mL and mixes evenly, and the gained mixture is carried out Ultrasonic treatment for 30min, followed by vacuum filtration, the filtration pressure is 0.1MPa, the filter membrane is cellulose membrane, the obtained product and the filter membrane are freeze-dried at -47°C for 12h, the product falls off from the filter membrane, and MXene / PS is obtained / SWCNTs composite film.

Embodiment 3

[0052] A preparation method of MXene-based three-dimensional porous flexible self-supporting membrane is as described in Example 1, the difference is: in step (2), 10mL styrene and 1.5mL acrylic acid are added to 150mL ultrapure water, and heated to 80°C , adding 9mL mass concentration of 1.0wt% ammonium persulfate (APS) aqueous solution, the addition rate of ammonium persulfate (APS) aqueous solution is 10min / mL, then react at 90°C for 24h; after the reaction is completed, filter, and use the obtained precipitate Washing with deionized water three times and drying to obtain polystyrene (PS) microspheres with uniform size; the particle diameter of the obtained PS microspheres is 0.2-0.3 μm.

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Abstract

The invention relates to an MXene-based three-dimensional porous flexible self-supporting membrane, a preparation method thereof and an application of the membrane in electrochemical adsorption of dyes. The preparation method of the self-supporting membrane comprises the following steps that an MXene nanosheet suspension, a polystyrene microsphere suspension and a single-walled carbon nanotube suspension are mixed and stirred to be uniform, an obtained mixed solution is subjected to ultrasonic treatment, then vacuum filtration is conducted, so that an MXene / PS / SWCNTs composite film is obtained, and then, the polystyrene microsphere template is removed, so that the MXene-based three-dimensional porous flexible self-supporting membrane can be obtained. The self-supporting membrane obtained in the invention has a large pore volume and a high specific surface area, and can expose more active sites. The prepared self-supporting membrane is used for removing dye through electrochemical adsorption and has the advantages of being high in removal efficiency, easy to recycle, low in cost, easy to control and the like.

Description

technical field [0001] The invention relates to an MXene-based three-dimensional porous flexible self-supporting membrane, a preparation method thereof and an application in electrochemically adsorbing dyes, belonging to the technical field of composite materials. Background technique [0002] MXenes are a new type of two-dimensional transition metal nitrides, carbides or carbonitrides. The preparation of MXenes is mainly produced by etching the "A" layer in the MAX phase of the ternary layered transition metal carbide with hydrofluoric acid (HF), or a mixed solution of hydrochloric acid (HCl) and lithium fluoride (LiF), where " M" stands for transition metals, such as (Ti, V, Sc, Cr, Zr, etc.); "A" stands for Al, Sn, etc.; X is C or N. The general chemical formula of MXenes is M n+1 x n T x , where n is a natural constant of 1-3, T x is the surface functional group (such as O, OH, F, NH 3 , NH 4 Wait). Due to their unique structure, MXenes have high electrical condu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30C01B32/168C01B32/921B01D69/12B01D67/00C02F1/469C02F101/30
CPCB01J20/20B01J20/0211B01J20/28033C01B32/921C01B32/168B01D69/12B01D67/0039C02F1/469C01P2004/80B01J2220/4812B01J2220/4806B01J2220/42C02F2101/308
Inventor 侯士峰姚晨雪
Owner SHANDONG UNIV
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