CN116395692A - In-plane porous MXene nano-sheet and preparation method and application thereof - Google Patents
In-plane porous MXene nano-sheet and preparation method and application thereof Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 41
- 230000003647 oxidation Effects 0.000 claims abstract description 23
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000005530 etching Methods 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000001179 sorption measurement Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- 238000010612 desalination reaction Methods 0.000 claims abstract description 5
- 238000000746 purification Methods 0.000 claims abstract description 5
- 239000013535 sea water Substances 0.000 claims abstract description 5
- 239000010865 sewage Substances 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- 239000002064 nanoplatelet Substances 0.000 claims description 25
- 238000005119 centrifugation Methods 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 10
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005273 aeration Methods 0.000 description 3
- 238000005276 aerator Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000004080 punching Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses an in-plane porous MXene nano-sheet, and a preparation method and application thereof. The preparation method comprises the following steps: (1) preparing an MXene nano-sheet solution by a chemical stripping method; (2) Oxidizing and etching the MXene nano-sheet solution by using an ozone generator; (3) And (2) adding HF into the solution subjected to ozone oxidation etching treatment in the step (2), dissolving an oxidation product on the surface of the MXene nano-sheet, centrifugally washing the reacted solution for a plurality of times until the pH value is 4-6, and performing ultrasonic dispersion to obtain the in-plane porous MXene nano-sheet solution. The preparation method disclosed by the invention is simple in process, green and mild in temperature and low in cost, the pore size of the obtained in-plane porous MXene nano-sheet material is adjustable, the pore size distribution is uniform, and the porous MXene nano-sheet material has a large specific surface area and rich active sites, so that the porous MXene nano-sheet material has a wide application prospect in the fields of gas separation, sea water desalination, ion adsorption, sewage purification and the like.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to an in-plane porous MXene nano-sheet, and a preparation method and application thereof.
Background
Since 2011 two-dimensional transition metal carbide or nitride (mxnes) materials were discovered, due to their unique atomic thickness, adjustable lateral dimensions, excellent mechanical properties, and abundant surface chemical groups, they have been widely used in environmental fields such as gas separation, sea water desalination, ion adsorption, sewage purification, and the like.
Mxnes has the disadvantage of ultra-thin two-dimensional materials, in particular a strong tendency to overlap, and lacks a limited porous structure. These problems can reduce surface active sites, provide long and tortuous transport paths between layers, hinder adsorption and transport of ions and gases, and limit the payload of other functional materials, resulting in undesirable performance. To address this problem, researchers have focused on providing more transport channels and more adsorption sites by manually introducing in-plane nanopores on two-dimensional nanoplates. Few MXene nano-platelet in-plane pore-forming strategies have appeared at present, mainly comprising Cu 2+ 、H 2 O 2 The oxidation and n-butylamine intercalation thermal shock methods often need to introduce pollutant substances, and the pore diameter is overlarge due to excessive oxidation and etching, so that development of a simple, green and mild MXene punching method for preparing the MXene material with adjustable pore diameter (from Emi to nm) and uniform pore distribution is urgently needed.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the primary purpose of the invention is to provide a preparation method of an in-plane porous MXene nano-sheet. The preparation method utilizes ozone to oxidize and etch the MXene nano-sheet to prepare the MXene material with adjustable pore size (from Emi to nm) and uniform pore distribution. The specific punching mechanism is as follows: ozone molecules are capable of rearranging and migrating functional groups on the surface of MXene and are CO or CO-based 2 Form vacancies, and can oxidize M atoms, further forming pores by dissolving oxidation products of the MXene surface. The preparation method is green and mild, has low cost, and widens the application of the MXene material
The second object of the present invention is to provide the in-plane porous MXene nano-sheet prepared by the preparation method.
A third object of the present invention is to provide the use of the above-described in-plane porous MXene nanoplatelets.
The primary object of the invention is achieved by the following technical solutions,
the preparation method of the in-plane porous MXene nano-sheet comprises the following steps:
(1) Preparing an MXene nano-sheet solution by a chemical stripping method;
(2) Oxidizing and etching the MXene nano-sheet solution by using an ozone generator;
(3) And (2) adding HF into the solution subjected to ozone oxidation etching treatment in the step (2), dissolving an oxidation product on the surface of the MXene nano-sheet, centrifugally washing the reacted solution for a plurality of times until the pH value is 4-6, and performing ultrasonic dispersion to obtain the in-plane porous MXene nano-sheet solution.
Preferably, the MXene nanoplatelets in step (1) are Ti 3 C 2 T x 、Ti 2 CT x 、V 2 CT x 、Mo 2 CT x 、Nb 2 CT x 、Nb 4 C 3 T x At least one of them.
Preferably, the mass concentration of ozone generated by the ozone generator in the step (2) is 10-80mg/L, and the oxidation time of the MXene nano-sheet solution is 30s-5min.
Preferably, the mass concentration of the MXene nano-sheet solution in the step (2) is 0.5-1.5mg/mL.
Wherein, the ozone generator in the step (2) is commercially available, and the concentration of ozone can be controlled by adjusting the current and the oxygen flow. Ozone generated by the ozone generator enters the MXene nanosheet solution through an aeration pipe, and an aeration head of the aeration pipe is a columnar sand core.
Preferably, the mass concentration of the HF in the solution subjected to the ozone oxidation etching treatment in the step (3) is 5-20%, and the dissolution time is 5-30min.
Preferably, the rotational speed of the centrifugation in the step (3) is 8000-10000rpm, the centrifugation time is 5-30min, the centrifugation times are 3-5 times, the ultrasonic power is 200-400W, and the time is 10-30min.
The second object of the invention is achieved by the following technical scheme:
an in-plane porous MXene nano-sheet is prepared by the preparation method.
The third object of the invention is achieved by the following technical scheme:
an application of an in-plane porous MXene nano-sheet in the fields of gas separation, sea water desalination, ion adsorption and sewage purification.
Compared with the prior art, the invention has the following beneficial effects:
(1) The method utilizes ozone to carry out oxidation etching treatment on the two-dimensional MXene nano-sheet solution to prepare the in-plane porous MXene nano-sheet, the ozone is more green and mild compared with other punching methods, the method is simple and easy to expand, the prepared aperture range is wide (from Emi to nm), and the pore distribution is uniform.
(2) The in-plane porous MXene nano-sheet prepared by the method increases the specific surface area and the active site of the MXene material, improves the problem of stacking the MXene nano-sheet, and can shorten the interlayer transportation path, so that the method can be better applied to the fields of gas separation, sea water desalination, ion adsorption, sewage purification and the like.
Drawings
FIG. 1 is a TEM image of an in-plane porous MXene nanoplatelet prepared in example 1;
FIG. 2 is an SEM image of an in-plane porous MXene nanoplatelet prepared according to example 2;
FIG. 3 is an SEM image of an in-plane porous MXene nanoplatelet prepared in example 3;
FIG. 4 is an SEM image of a porous MXene nanoplatelet prepared according to comparative example 1;
FIG. 5 is an SEM image of porous MXene nanoplatelets prepared in comparative example 3.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
Example 1
An in-plane porous MXene nanoplatelet comprising the steps of:
(1) MXene (Ti) is prepared by chemical stripping method 3 C 2 T x ) The nano-sheet solution comprises the following specific steps: 2.5g of lithium fluoride、2g Ti 3 AlC 2 Mixing the powder with 9M 50ml hydrochloric acid solution, stirring at 50deg.C for 30 hr, repeatedly centrifuging and washing at 3500rpm until pH is about 6, dispersing the product into water again, ultrasonically treating under argon protection atmosphere for 20min, centrifuging at 3500rpm for 1 hr, and collecting supernatant to obtain Ti 3 C 2 T x A nanoplatelet solution;
(2) Adjusting the current and the oxygen flow of an ozone generator, controlling the ozone concentration to be 10mg/L, and carrying out oxidation etching treatment on 60mL of 1.5mg/L MXene nano-sheet solution by ozone through an aerator pipe for 30s;
(3) And (2) adding 5% HF into the solution prepared in the step (2) to dissolve an oxidation product on the surface of the MXene, centrifuging and washing the reacted solution at 8000rpm for 10min, repeating the centrifugation for several times until the pH value is 6, and further performing ultrasonic dispersion at 200W for 10min to obtain the in-plane porous MXene nano-sheet solution.
As shown in TEM of FIG. 1, certain nanopores and Emi pores (marked by white dotted lines) exist on the surface of the MXene nanoplatelets after 30s of ozone oxidation treatment.
Example 2
An in-plane porous MXene nanoplatelet comprising the steps of:
(1) MXene (Ti) is prepared by chemical stripping method 3 C 2 T x ) Nanoplatelet solutions (same as example 1);
(2) Adjusting the current and the oxygen flow of an ozone generator, controlling the ozone concentration to be 40mg/L, and carrying out oxidation etching treatment on 60mL of 1mg/L MXene nanosheet solution by ozone through an aerator pipe for 1min;
(3) And (2) adding 5% HF into the solution prepared in the step (2) to dissolve an oxidation product on the surface of the MXene, centrifuging and washing the reacted solution at 8000rpm for 10min, repeating the centrifugation for several times until the pH value is 6, and further performing ultrasonic dispersion at 200W for 10min to obtain the in-plane porous MXene nano-sheet solution.
As shown in FIG. 2, the surface of the MXene nano-sheet subjected to ozone oxidation treatment for 1min has pore diameters of several to tens of nm, but the pore density is too small.
Example 3
An in-plane porous MXene nanoplatelet comprising the steps of:
(1) MXene (Ti) is prepared by chemical stripping method 3 C 2 T x ) Nanoplatelet solutions (same as example 1);
(2) Adjusting the current and the oxygen flow of an ozone generator, controlling the ozone concentration to be 40mg/L, and carrying out oxidation etching treatment on 60mL of 1mg/L MXene nanosheet solution by ozone through an aerator pipe for 5min;
(3) And (2) adding 5% HF into the solution prepared in the step (2) to dissolve an oxidation product on the surface of the MXene, centrifuging and washing the reacted solution at 8000rpm for 10min, repeating the centrifugation for several times until the pH value is 6, and further performing ultrasonic dispersion at 200W for 10min to obtain the in-plane porous MXene nano-sheet solution.
As shown in FIG. 3, the surface of the MXene nano-sheet subjected to ozone oxidation treatment for 5min has pore diameters of several to several hundred nm, and the pore density is larger.
Comparative example 1
The difference from example 1 is that there is no difference to Ti 3 C 2 T x The nano-sheet is subjected to ozone etching for pore-forming, and MXene (Ti) is prepared only by chemical stripping 3 C 2 T x ) Nanosheet solution (same as in example 1).
As shown in FIG. 4, the MXene nanoplatelets after chemical stripping were smooth in surface and were free from defects.
Comparative example 2
The difference from example 1 is that only the ratio of Ti was changed 3 C 2 The concentration of ozone for pore-forming of Tx nanoplatelets was 5mg/L, otherwise the same as in example 1.
The MXene nano-sheets treated by the low-dose ozone concentration are same as the original MXene nano-sheets, and the surface is flat and has no defects.
Comparative example 3
The difference from example 1 is that only the ratio of Ti was changed 3 C 2 T x The ozone concentration of the nanosheets for pore-forming was 100mg/L, and the other methods were the same as in example 1.
As shown in FIG. 5, the morphology of the MXene nanoplatelets after high dose ozone concentration treatment has been completely destroyed.
The following is experimental verification data in gas separation for the MXene membranes prepared in examples and comparative examples.
First, the MXene nanoplatelet solutions prepared in examples 1 to 3 and comparative examples 1 to 3 were deposited on a nylon substrate having a pore size of 0.22 μm and a diameter of 10cm by vacuum filtration, and dried in a vacuum oven at 60 ℃ for 12 hours to obtain a two-dimensional MXene film. Placing a two-dimensional MXene membrane into a gas separation device, and introducing H at the feeding side 2 /CO 2 The volume ratio of the mixture (flow rate: 50 mL/min) was 1:1, and the mixture was detected by purging argon (flow rate: 50 mL/min) and gas chromatography, and the gas separation performance was shown in Table 1:
as can be seen from Table 1, the MXene film prepared in comparative example 1 has higher selectivity, but H 2 The permeation rate is low due to the fact that gas molecules can only be transported through the MXene interlayer without additional gas transport channels. By comparing the separation performance of examples 1, 2 and 3, it was demonstrated that H as the ozone concentration increased 2 The permeation rate is obviously improved, and the interlayer transmission distance is shortened due to the fact that the gas transmission channel is increased in the surface inner hole on the MXene nano-sheet; the slightly reduced selectivity, but still maintained at a better separation performance, is mainly due to the pores on the nanoplatelets, although larger than the molecular kinetic diameter of the gas, the MXene interlayer spacing is between H 2 /CO 2 Can realize gas sieving. In addition, the MXene film prepared by comparative example 2 has similar properties to the original MXene film without ozone treatment, demonstrating that the lower dosage of ozone concentration does not allow for pore-forming of the MXene nanoplatelets. The MXene film prepared by comparative example 3 although exhibiting higher H 2 The permeation rate, but little selectivity, demonstrated that higher doses of ozone concentration severely destroyed the MXene nanoplatelet structure, resulting in poor membrane separation performance.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (8)
1. The preparation method of the in-plane porous MXene nano-sheet is characterized by comprising the following steps of:
(1) Preparing an MXene nano-sheet solution by a chemical stripping method;
(2) Oxidizing and etching the MXene nano-sheet solution by using an ozone generator;
(3) And (2) adding HF into the solution subjected to ozone oxidation etching treatment in the step (2), dissolving an oxidation product on the surface of the MXene nano-sheet, centrifugally washing the reacted solution for a plurality of times until the pH value is 4-6, and performing ultrasonic dispersion to obtain the in-plane porous MXene nano-sheet solution.
2. The method of claim 1, wherein in step (1), the MXene nanoplatelets are Ti 3 C 2 T x 、Ti 2 CT x 、V 2 CT x 、Mo 2 CT x 、Nb 2 CT x 、Nb 4 C 3 T x At least one of them.
3. The method for preparing an in-plane porous MXene nano-sheet according to claim 1, wherein the mass concentration of ozone generated by the ozone generator in the step (2) is 10-80mg/L, and the oxidation time of the MXene nano-sheet solution is 30s-5min.
4. The method for preparing an in-plane porous MXene nano-sheet according to claim 1, wherein the mass concentration of the MXene nano-sheet solution in the step (2) is 0.5-1.5mg/mL.
5. The method for preparing an in-plane porous MXene nano-sheet according to claim 1, wherein the mass concentration of HF in the solution treated by ozone oxidation etching in the step (3) is 5-20%, and the dissolution time is 5-30min.
6. The method for preparing an in-plane porous MXene nano-sheet according to claim 1, wherein the rotational speed of centrifugation in the step (3) is 8000-10000rpm, the centrifugation time is 5-30min, the centrifugation times are 3-5 times, the ultrasonic power is 200-400W, and the time is 10-30min.
7. An in-plane porous MXene nanoplatelet prepared according to the method of any one of claims 1 to 6.
8. Use of the in-plane porous MXene nanoplatelets according to claim 7 in the field of gas separation, sea water desalination, ion adsorption and sewage purification.
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| THIERRY K SLOT等: "Surface oxidation of Ti3C2Tx enhances the catalytic activity of supported platinum nanoparticles in ammonia borane hydrolysis", 《2D MATER》, 6 October 2020 (2020-10-06), pages 1 - 9 * |
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