CN111704137A - Preparation method of high-yield low-fluorine-content few-layer MXenes nanosheet - Google Patents
Preparation method of high-yield low-fluorine-content few-layer MXenes nanosheet Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims abstract description 16
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 14
- 239000011737 fluorine Substances 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000005416 organic matter Substances 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- MATGKVZWFZHCLI-LSDHHAIUSA-N (-)-matairesinol Chemical compound C1=C(O)C(OC)=CC(C[C@@H]2[C@H](C(=O)OC2)CC=2C=C(OC)C(O)=CC=2)=C1 MATGKVZWFZHCLI-LSDHHAIUSA-N 0.000 abstract description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 abstract description 4
- -1 polyoxyethylene Polymers 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002055 nanoplate Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000012983 electrochemical energy storage Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
A preparation method of a few-layer MXenes nanosheet with high yield and low fluorine content belongs to the technical field of nano materials. Mixing organic matters containing hydroxyl or active oxygen such as polyethylene glycol or alkylphenol polyoxyethylene, MAX, hydrochloric acid and lithium fluoride, stirring at 35 ℃ for 24 hours, washing with water until PH is neutral, and centrifuging to obtain the low-fluorine-content MXenes nanosheet. The invention effectively solves a series of problems of low yield and high fluorine content in the preparation process of the few-layer MXenes nanosheets, and has the advantages of simple preparation method, low price, large-scale production and practical prospect.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a high-yield low-fluorine-content few-layer MXenes nanosheet.
Background
The transition metal carbide MXenes is a novel two-dimensional material with a graphene-like structure, and has the advantages of good chemical stability, hydrophilicity, conductivity, mechanical property, high specific surface area and the like. Since the discovery of the Yury GogotSi and the like in 2011, the method has shown great application prospects in the fields of electrochemical energy storage, sewage treatment, sensors, seawater desalination and the like. At present, MXenes is prepared by etching a weaker A-site element in a MAX phase by using a mixed solution of hydrofluoric acid or villiaumite and hydrochloric acid. MXenes materials prepared by the method often have functional groups such as F, OH, O and the like, and the yield of the MXenes nanosheets prepared by stripping is extremely low. More seriously, the application of MXenes nanosheets, especially in electrochemical energy storage, is hindered by the presence of a large number of F functional groups. Therefore, the exploration of a method for preparing MXenes nanosheets with high yield and low fluorine content through improving chemical etching is the key of further industrial application of the method.
Disclosure of Invention
The invention aims to: the method provides a simple and improved process for preparing the low-fluorine-content few-layer MXenes nanosheet, and improves the yield of the low-layer MXenes, so as to solve the problems of high fluorine content and low yield of the MXenes nanosheet in the conventional preparation method.
The method comprises the steps of mixing organic matters containing hydroxyl or active oxygen such as polyethylene glycol or alkylphenol ethoxylates, MAX, hydrochloric acid and lithium fluoride, stirring at 35 ℃ for 24 hours, washing with water until the PH is neutral, and centrifuging to obtain the low-fluorine-content MXenes nanosheet. In the stirring and etching process, a large amount of hydroxyl or active oxygen on the molecular chain of organic matter containing hydroxyl or active oxygen, such as polyethylene glycol or alkylphenol polyoxyethylene can be rapidly combined with Ti atoms to form a stable structure, so that the possibility of combining F atoms with titanium is reduced, and further, the preparation of the MXenes nanosheets with low fluorine content is realized. In addition, organic molecules containing hydroxyl or active oxygen, such as long-chain polyethylene glycol or alkylphenol ethoxylates, are also used as an intercalating agent between MXenes lamellae, so that the van der Waals force between the lamellae is reduced, the peeling speed of the lamellae is accelerated, and the yield is improved.
The specific preparation process comprises the following steps:
(1) mixing organic substance containing hydroxyl or active oxygen such as polyethylene glycol or alkylphenol polyoxyethylene, hydrochloric acid, and lithium fluoride
Wherein, the proportion of organic matters containing hydroxyl or active oxygen such as polyethylene glycol or alkylphenol polyoxyethylene in the mixed solvent is 1-5%;
(2) adding MAX into the mixed solution obtained in the step (1) slowly, and stirring for 24 hours at 35 ℃;
(3) mechanically shaking the product obtained in the step (2) for 20-60min, then washing with water until the pH value is neutral, and centrifuging to obtain the few-layer MXenes nanosheet with low fluorine content.
Wherein the organic matter containing hydroxyl or active oxygen accounts for 1-5 wt% of the mixed solvent.
The specifications of the alkylphenol polyoxyethylene ether in the invention comprise OP-4, OP-7, OP-10 or OP-15, and the molecular formula is C34H62O11。
The invention effectively solves a series of problems of low yield and high fluorine content in the preparation process of the few-layer MXenes nanosheets, and has the advantages of simple preparation method, low price, large-scale production and practical prospect.
Drawings
Fig. 1 is a scanning electron microscope image of the few-layer MXenes nanosheets prepared in example 1.
Figure 2 is an XRD of the few-layer MXenes nanoplates prepared in example 1.
Figure 3 is a comparison of the F content of few-layered MXenes nanoplates prepared in example 1 with a conventional sample.
Figure 4 is a comparison of the yield of few-layered MXenes nanoplates prepared in example 1 to a conventional sample.
Detailed Description
Example 1:
(1) adding 1g of polyethylene glycol and 1g of lithium fluoride into 20ml of 9M hydrochloric acid, and uniformly mixing;
(2) MAX with the mass of 1g is slowly added to the mixed solution obtained in the step (1), and stirred at the temperature of 35 ℃ for 24 hours.
(3) Mechanically shaking the product obtained in the step (2) for 20-60min, then washing with water until the pH value is neutral, and centrifuging to obtain the few-layer MXenes nanosheet with low fluorine content.
Example 2:
(1) adding 1g of lithium fluoride and 1gOP-4 with mass into 20ml of 9M hydrochloric acid, and uniformly mixing;
(2) MAX with the mass of 1g is slowly added to the mixed solution obtained in the step (1), and stirred at the temperature of 35 ℃ for 24 hours.
(3) Mechanically shaking the product obtained in the step (2) for 20-60min, then washing with water until the pH value is neutral, and centrifuging to obtain the few-layer MXenes nanosheet with low fluorine content.
Example 3:
(1) adding 1g of lithium fluoride and 1gOP-10 mass parts into 20ml of 9M hydrochloric acid, and uniformly mixing;
(2) MAX with the mass of 1g is slowly added to the mixed solution obtained in the step (1), and stirred at the temperature of 35 ℃ for 24 hours.
(3) Mechanically shaking the product obtained in the step (2) for 20-60min, then washing with water until the pH value is neutral, and centrifuging to obtain the few-layer MXenes nanosheet with low fluorine content.
Comparative example 1
(1) Adding 1g of lithium fluoride into 20ml of 9M hydrochloric acid, and uniformly mixing;
(2) MAX with the mass of 1g is slowly added to the mixed solution obtained in the step (1), and stirred at the temperature of 35 ℃ for 24 hours.
(3) Mechanically shaking the product obtained in the step (2) for 20-60min, then washing with water until the pH value is neutral, and centrifuging to obtain the few-layer MXenes nanosheet with low fluorine content.
SEM, XRD and XPS tests are carried out on the obtained few-layer MXenes with low fluorine content, and the few-layer MXenes nanosheets prepared by the SEM and XRD result improving process are not different from samples prepared by the conventional process, as shown in figures 1 and 2. However, XPS test shows that the fluorine content of the sample obtained by the improved process is obviously reduced, and the yield is greatly improved, as shown in figures 3 and 4.
Claims (4)
1. A preparation method of a few-layer MXenes nanosheet with high yield and low fluorine content is characterized by comprising the following steps: the preparation method comprises the following steps of,
1) mixing an organic matter containing hydroxyl or active oxygen, hydrochloric acid and lithium fluoride;
2) adding MAX into the mixed solution obtained in the step (1) slowly, and stirring for 24 hours at 35 ℃;
3) mechanically shaking the product obtained in the step 2) for 20-60min, then washing with water until the pH value is neutral, and centrifuging to obtain the low-fluorine-content few-layer MXenes nanosheet.
2. The method for preparing the high-yield low-fluorine-content few-layer MXenes nanosheets of claim 1, wherein: the organic matter containing hydroxyl or active oxygen in the step 1) is polyethylene glycol or alkylphenol ethoxylates.
3. The method for preparing the high-yield low-fluorine-content few-layer MXenes nanosheets of claim 2, wherein: the organic substance of alkylphenol polyoxyethylene ether includes OP-4, OP-7, OP-10 or OP-15.
4. The method for preparing high-yield low-fluorine-content few-layer MXenes nanosheets as claimed in claim 1 or 2, wherein: the organic matter containing hydroxyl or active oxygen accounts for 1-5 wt% of the mixed solvent.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244388A (en) * | 2018-08-20 | 2019-01-18 | 同济大学 | Covalent organic framework/titanium carbide nanosheet composite material preparation and application |
| CN109666964A (en) * | 2019-01-16 | 2019-04-23 | 华南理工大学 | A kind of method that electrophoretic deposition quickly prepares two-dimentional MXene film |
| CN109694074A (en) * | 2019-03-04 | 2019-04-30 | 青岛大学 | A kind of method that electrochemical process prepares MXenes and its derivates nanometer piece |
| CN110615440A (en) * | 2019-09-24 | 2019-12-27 | 黑龙江科技大学 | MXene nanosheet with large size and rich oxygen functional group and preparation method and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244388A (en) * | 2018-08-20 | 2019-01-18 | 同济大学 | Covalent organic framework/titanium carbide nanosheet composite material preparation and application |
| CN109666964A (en) * | 2019-01-16 | 2019-04-23 | 华南理工大学 | A kind of method that electrophoretic deposition quickly prepares two-dimentional MXene film |
| CN109694074A (en) * | 2019-03-04 | 2019-04-30 | 青岛大学 | A kind of method that electrochemical process prepares MXenes and its derivates nanometer piece |
| CN110615440A (en) * | 2019-09-24 | 2019-12-27 | 黑龙江科技大学 | MXene nanosheet with large size and rich oxygen functional group and preparation method and application thereof |
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