CN113041855A - Two-dimensional porous MXene film and preparation method and application thereof - Google Patents
Two-dimensional porous MXene film and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002135 nanosheet Substances 0.000 claims abstract description 57
- 239000012528 membrane Substances 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000011148 porous material Substances 0.000 claims abstract description 14
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 32
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 229960003638 dopamine Drugs 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 15
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- 238000005530 etching Methods 0.000 claims description 11
- 239000007983 Tris buffer Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000002064 nanoplatelet Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 239000012510 hollow fiber Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- 230000004907 flux Effects 0.000 abstract description 16
- 239000000975 dye Substances 0.000 abstract description 13
- 230000005540 biological transmission Effects 0.000 abstract description 6
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- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 11
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
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- 229910021389 graphene Inorganic materials 0.000 description 2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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- Water Supply & Treatment (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a two-dimensional porous MXene membrane and a preparation method and application thereof. The preparation method comprises the steps of firstly preparing the porous MXene nanosheets by using a chemical etching method, and then assembling the prepared porous MXene nanosheets onto a support body by using a pressure auxiliary method to obtain the two-dimensional porous MXene membrane. According to the invention, artificial pore is introduced on the surface of the MXene nanosheet through a simple chemical etching method, a transmission model of water molecules in the membrane is changed, a transmission channel of the water molecules in the membrane is increased, the average transmission distance of the water molecules in the membrane is shortened, an effective molecular screening pore channel between layers of the two-dimensional MXene membrane is effectively reserved, the water flux of the membrane is greatly increased, and meanwhile, the high retention performance of the membrane on small molecular dyes is reserved. The preparation method is simple in preparation process, good in controllability, strong in expandability, green and environment-friendly, and is a novel and efficient method for preparing the two-dimensional MXene base film in the high-performance water treatment field.
Description
Technical Field
The invention belongs to the technical field of preparation of membranes, and particularly relates to a two-dimensional porous MXene membrane and a preparation method and application thereof.
Background
Water is the source of all earth's life and one of the important material resources on which human beings live and develop. The development of social economy benefits mankind and simultaneously generates a series of water pollution problems. And because the per capita water resource ratio of China is small, the demand for drinking water is increasing day by day, and the research and development of high-efficiency water treatment technology not only has important strategic significance, but also has important practical significance.
Compared with the traditional separation technology, the application of the membrane separation technology in water treatment has the advantages of energy conservation, high efficiency, environmental protection and the like. Therefore, research and development of high performance membranes has been a goal of researchers. In recent years, two-dimensional layered membranes assembled from ultra-thin two-dimensional materials have been favored by many researchers because of the order and controllability of the nanochannels between the layers and the theoretically minimum transport resistance, and are expected to achieve excellent performance in water treatment. Recently, a novel two-dimensional nanomaterial MXene (Ti)3C2Tx) Relative to other two-dimensional materials such as: graphene and graphene oxide have unique advantages such as: high thermal stability, good structural stability in aqueous solutions, and the like. In the practical application process, however, the MXene membrane layers have narrow intervals, so that the permeability is low. In addition, in order to support the two-dimensional nanomaterial on the surface of the support carrier, calcination is usually performed to tightly bond the two-dimensional nanomaterial of the separation layer to the support layer, but the calcination process also causes damage and change in the microstructure of the material of the separation layer.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: (1) improving the water flux of the separation membrane loaded with MXene; (2) the bonding force between the film layer and the substrate is ensured under the condition of no calcination; the invention aims to provide a two-dimensional porous MXene film, and the invention also aims to provide a preparation method of the two-dimensional porous MXene film; it is also an object of the invention to provide the use of the two-dimensional porous MXene film. The porous MXene membrane prepared by the method has high water flux and continuous and efficient small-molecule dye retention.
The technical scheme of the invention is as follows: the artificial pore is introduced on the surface of the MXene nanosheet through a simple chemical etching method, a transmission model of water molecules in the membrane is changed, transmission channels of the water molecules in the membrane are increased, the average transmission distance of the water molecules in the membrane is shortened, the water flux of the membrane is greatly increased, effective molecular screening pore channels between layers of the two-dimensional MXene membrane are effectively reserved, and meanwhile the high retention performance of the membrane on small molecular dyes is realized. Therefore, the method is simple in preparation process, good in controllability, strong in expandability, green and environment-friendly, and is a novel and efficient method for preparing the two-dimensional MXene base film in the high-performance water treatment field.
The specific technical scheme of the invention is as follows: the two-dimensional porous MXene membrane is characterized by comprising a modified support body and a modification layer, wherein the modification layer is coated on the surface of the modified support body, the modification layer is a porous MXene nanosheet obtained through hydrogen peroxide treatment, and the modified support body is polydopamine-modified porous ceramic.
The invention also provides a method for preparing the two-dimensional porous MXene membrane, which comprises the following specific steps:
(1) preparation of porous MXene nanosheet: stirring MXene nanosheet and dispersing into hydrogen peroxide (H) with certain mass concentration2O2) Stirring and etching the solution for a certain time at a certain temperature, centrifuging and washing the reacted solution, and performing ultrasonic dispersion to obtain the product with the concentration of 0.001-0.005 mg/mL-1Porous MXene nanosheet solution.
(2) Preparing a modified support body: preparing a mixed solution of dopamine and Tris (hydroxymethyl) methylamine (Tris), wherein the concentrations of the dopamine and the Tris are 0.5-5 mg/mL respectively-1And 2-25mM, soaking the porous support in the mixed solution, depositing dopamine for 5-30h, cleaning the modified porous support, and drying.
(3) Assembling the prepared porous MXene nanosheets on a modified support body layer by a filter pressing method or a vacuum suction method, then drying the wet film in vacuum to obtain a two-dimensional porous MXene film, and controlling the loading capacity of the porous MXene nanosheets to be 107-182 mg/m-2。
Preferably MXene nanosheets are Ti3C2TxOther MXene nanoplates are also suitable.
Preferred MXene nanosheets and H2O2In a mass ratio of 0.2 to 1, H2O2The mass fraction of the solution is 0.01-0.07%.
The preferred etching temperature is 20-60 ℃, and the etching time is 10-80 min.
The assembly pressure of the porous MXene nanosheets is preferably 0.1-0.5 MPa. The preferred porous support is a sheet type, single tube or hollow fiber porous ceramic material, and the preferred average pore diameter of the porous support is 80-400 nm.
Preferably, the drying temperature of wet film vacuum drying is 40-100 ℃, and the drying time is 3-12 h.
The invention also provides application of the two-dimensional porous MXene membrane in dye solution filtration. The two-dimensional porous MXene membrane is applied to filtering dye solution.
Has the advantages that:
1. by means of H2O2The mild chemical etching introduces artificial pores on the surface of the MXene nanosheets, and the method has the advantages of simplicity, controllability, greenness, easiness in expansion and the like, and provides guarantee for the subsequent preparation of the high-performance porous MXene film.
2. A large number of manholes are introduced into the surface of the MXene nanosheet, so that the water flux of the MXene membrane is greatly improved.
3、H2O2While introducing artificial pores on the surface of the MXene nanosheets, the mild chemical etching well preserves the two-dimensional sheet structure of the original nanosheets, so that effective molecular screening pore channels between the MXene two-dimensional layers are well reserved, and the efficient interception of the micromolecular dye is realized.
4. The bonding force between the MXene nanosheets and the supporting layer is improved by utilizing the polymerization of dopamine, and the calcining treatment is not required.
Drawings
Fig. 1 is SEM image of porous MXene nanosheets of example 1.
FIG. 2 is a SEM image of the surface of a porous MXene film in example 1.
Fig. 3 is a raman spectrum of the porous MXene nanosheet of example 1.
Fig. 4 is an SEM image of MXene nanoplatelets in comparative example 1.
FIG. 5 is a schematic view of a porous MXene membrane in comparative example 1.
Fig. 6 is SEM image of porous MXene nanosheets of example 2.
FIG. 7 is a SEM image of a cross section of a porous MXene film in example 3.
Fig. 8 is an infrared spectrum of the porous MXene film of example 3.
Detailed Description
Example 1
(1) Preparation of porous MXene nanosheet: taking MXene (Ti)3C2Tx) Stirring and dispersing the nano-sheets to 0.02 wt% of hydrogen peroxide (H)2O2) Medium, MXene nano sheet and H2O2Is 0.5, is stirred and etched at 25 ℃ for 30min, and then the solution after reaction is centrifugally washed to obtain 0.002 mg.mL-1Porous MXene nano-sheet
(2) Preparing a modified support body: preparing a mixed solution of dopamine and Tris (hydroxymethyl) methylamine (Tris), wherein the concentrations of the dopamine and the Tris are respectively 2 mg-mL-1And 10mM, soaking the single-tube ceramic support body with the aperture of 100nm in the mixed solution, depositing dopamine for 20 hours, and cleaning and drying the modified porous support body.
(3) Assembling the prepared porous MXene nanosheets layer by layer on the inner surface of a polydopamine-modified 100 nm-aperture single-tube ceramic support body under the pressure of 0.1Mpa by a filter pressing method or a vacuum suction method, and then drying the wet film at 80 ℃ in vacuum for 12 hours to obtain a two-dimensional porous MXene film, wherein the loading capacity of the porous MXene nanosheets is 108.7mg/m2。
FIG. 1 is SEM image of porous MXene nanosheets, and H can be seen from the SEM image2O2After mild etching, a large number of holes appear on the surface of the MXene nanosheet, and the two-dimensional morphology of the nanosheet is still maintained. FIG. 2 is a SEM image of the surface of a porous MXene film, wherein the SEM image shows that the film surface is complete and free of defects, meanwhile, the film surface is obviously formed by stacking a plurality of MXene nanosheets layer by layer, and more importantly, a large number of artificial pores can be obviously seen on the film surface, which shows that the MXene nanosheets areWas successfully introduced into the membrane. FIG. 3 is a Raman spectrum of the film. The prepared membrane is subjected to pure water flux test by adopting cross-flow filtration under the pressure of 0.5Mpa, and the pure water flux is 21.93L/(m2H.bar), the rejection of 10ppm of an aqueous solution of Congo Red (CR) dye was tested, and the rejection of congo red by the two-dimensional porous MXene membrane was 100%.
Comparative example 1
The difference from example 1 is that MXene (Ti) is not present3C2Tx) The nanosheet surface being bound by H2O2And etching and forming the hole.
MXene nanosheet dispersion (0.002 mg. mL)-1) Assembling the composite membrane layer by layer on the inner surface of a polydopamine-modified 100 nm-aperture single-tube ceramic support body by a pressure-assisted method, and drying the support body for 12 hours at 100 ℃ in vacuum to obtain a two-dimensional porous MXene membrane, wherein the loading capacity of MXene nanosheets is 108.7mg/m2。
Fig. 4 is a SEM image of MXene nanoplatelets, where the nanoplatelets can be seen to be thin and transparent. FIG. 5 is a solid view of a porous Mxeen membrane. The prepared membrane is subjected to pure water flux test by adopting cross-flow filtration under the pressure of 0.5Mpa, and the pure water flux is 9.37L/(m2H.bar), the rejection of 10ppm of an aqueous solution of Congo Red (CR) dye was tested, and the rejection of congo red by the two-dimensional porous MXene membrane was 100%.
In contrast to example 1, no H was passed2O2The retention rate of the MXene film for etching and pore forming to the dye is the same; but the water flux is very low, which shows that after MXene is treated by hydrogen peroxide in the scheme of the patent, the water flux of the composite membrane can be effectively improved, and the retention performance of the composite membrane on the dye is kept.
Example 2
(1) Preparation of porous MXene nanosheet: taking MXene (Ti)3C2Tx) Stirring and dispersing the nano-sheets to 0.05 wt% of hydrogen peroxide (H)2O2) Medium, MXene nano sheet and H2O2Is 1, is stirred and etched at 50 ℃ for 60min, and then the solution after reaction is centrifugally washed and redispersed to obtain 0.003 mg.mL-1Porous MXene nano-sheet
(2) Preparing a modified support body: preparing a mixed solution of dopamine and Tris (hydroxymethyl) methylamine (Tris), wherein the concentrations of the dopamine and the Tris are respectively 5mg & mL-1And (3) soaking the single-tube ceramic support body with the aperture of 300nm in the mixed solution for deposition of dopamine for 8 hours, and cleaning and drying the modified porous support body.
(3) Assembling the prepared porous MXene nanosheets layer by layer on the inner surface of a polydopamine-modified sheet-type ceramic support body with the aperture of 300nm by a filter pressing method or a vacuum suction method under the pressure of 0.4Mpa, and then drying the wet film at 60 ℃ in vacuum for 6 hours to obtain a two-dimensional porous MXene film, wherein the loading capacity of the porous MXene nanosheets is 181.2mg/m2。
Fig. 6 is a SEM image of porous MXene nanosheets, and it can be seen that a large number of large pores are formed on the surface of the nanosheets. The prepared membrane is subjected to pure water flux test by adopting cross-flow filtration under the pressure of 0.5Mpa, and the pure water flux is 60L/(m)2H.bar), the rejection of 10ppm of an aqueous solution of Congo Red (CR) dye was 80% for a two-dimensional porous MXene membrane. Compared with the example 1, the retention rate of the dye is reduced; but the water flux is extremely high, which shows that the effective molecular sieving pore channel of the membrane is enlarged when the hydrogen peroxide etching strength is very high in the scheme of the patent, so that the rejection rate of the membrane is reduced.
Example 3
(1) Preparation of porous MXene nanosheet: taking MXene (Ti)3C2Tx) Stirring and dispersing the nano-sheets to 0.02 wt% of hydrogen peroxide (H)2O2) Medium, MXene nano sheet and H2O2Is 0.5, is stirred and etched at 25 ℃ for 60min, and then the solution after the reaction is centrifugally washed to obtain 0.001 mg/mL-1Porous MXene nano-sheet
(2) Preparing a modified support body: preparing a mixed solution of dopamine and Tris (hydroxymethyl) methylamine (Tris), wherein the concentrations of the dopamine and the Tris are respectively 1mg & mL-1And (3) soaking the single-tube ceramic support body with the aperture of 100nm in the mixed solution for deposition of dopamine for 24 hours, and cleaning and drying the modified porous support body.
(3) Assembling porous MXene nanosheets layer by layer on the inner surface of a polydopamine-modified 100 nm-aperture single-tube ceramic support body under the pressure of 0.1Mpa by a filter pressing method or a vacuum suction method, and then drying the wet film at 100 ℃ in vacuum for 12 hours to obtain a two-dimensional porous MXene film, wherein the loading capacity of the porous MXene nanosheets is 108.7mg/m2. Fig. 7 is a cross-sectional SEM image of the porous MXene film, from which it can be seen that there is an obvious boundary layer between the film layer and the support, and the cross-sectional view clearly shows the morphology of the layer-by-layer stacking of MXene nanosheets. FIG. 8 is an infrared spectrum of the film, from which H can be seen2O2The surface before and after etching has no new functional groups generated. The prepared membrane is subjected to pure water flux test by adopting cross-flow filtration under the pressure of 0.5Mpa, and the pure water flux is 42.48L/(m2H.bar), the rejection of 10ppm of an aqueous solution of Congo Red (CR) dye was tested, and the rejection of congo red by the two-dimensional porous MXene membrane was 100%.
Claims (8)
1. The two-dimensional porous MXene membrane is characterized by comprising a modified support body and a modification layer, wherein the modification layer is coated on the surface of the modified support body, the modification layer is a porous MXene nanosheet obtained through hydrogen peroxide treatment, and the modified support body is polydopamine-modified porous ceramic.
2. A method for preparing the two-dimensional porous MXene membrane of claim 1, comprising the following steps:
(1) preparation of porous MXene nanosheet: stirring and dispersing MXene nanosheets into a hydrogen peroxide solution, stirring and etching for a certain time at a certain temperature, then centrifugally washing the reacted solution, and ultrasonically dispersing into deionized water to obtain a solution with the concentration of 0.001-0.005 mg/mL-1A porous MXene nanosheet solution;
(2) preparing a modified support body: preparing a mixed solution of dopamine and Tris (hydroxymethyl) methylamine (Tris), wherein the concentrations of the dopamine and the Tris are 0.5-5 mg/mL respectively-1And 2-25mM, soaking the porous support in the mixed solution, depositing dopamine for 5-30h, and mixingCleaning and drying the modified porous support body;
(3) assembling the prepared porous MXene nanosheets on a modified support body layer by a filter pressing method or a vacuum suction method, then drying the wet film in vacuum to obtain a two-dimensional porous MXene film, and controlling the loading capacity of the porous MXene nanosheets to be 107-182 mg/m-2。
3. The method of claim 2, wherein MXene nanoplatelets are associated with H2O2The mass ratio of (A) to (B) is 0.2-1; the mass fraction of the hydrogen peroxide solution is 0.01-0.07%.
4. The method according to claim 2, wherein the etching temperature is 20 to 60 ℃ and the etching time is 10 to 80 min.
5. The method according to claim 2, wherein the porous support is a sheet, a single tube or a hollow fiber porous material, and the average pore diameter of the porous support is 80 to 400 nm.
6. The method of claim 2, wherein the assembly pressure of the porous MXene nanosheets is 0.1 to 0.5 MPa.
7. The method according to claim 2, wherein the drying temperature of the wet film is 40-100 ℃ and the drying time is 3-12 h.
8. Use of the two-dimensional porous MXene membrane of claim 1 in dye solution filtration.
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| CN115096964A (en) * | 2022-07-26 | 2022-09-23 | 哈尔滨理工大学 | Electrochemical sensor based on MXene porous structure and preparation method and application thereof |
| CN115096964B (en) * | 2022-07-26 | 2024-04-05 | 哈尔滨理工大学 | Electrochemical sensor based on MXene porous structure and preparation method and application thereof |
| CN115676832A (en) * | 2022-11-25 | 2023-02-03 | 长沙新立硅材料科技有限公司 | Preparation method of cellulose-supported porous MXene material |
| CN116510531A (en) * | 2023-05-18 | 2023-08-01 | 宁夏大学 | High-permeation flux MXene/SiC ceramic composite nanofiltration membrane for dye separation and preparation method thereof |
| CN116510531B (en) * | 2023-05-18 | 2024-02-27 | 宁夏大学 | High-permeation flux MXene/SiC ceramic composite nanofiltration membrane for dye separation and preparation method thereof |
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