CN109701397B - Application of two-dimensional MXene membrane prepared by electrophoretic deposition method in ion interception - Google Patents
Application of two-dimensional MXene membrane prepared by electrophoretic deposition method in ion interception Download PDFInfo
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Abstract
The invention belongs to the technical field of ion interception, and discloses an application of a two-dimensional MXene membrane prepared by an electrophoretic deposition method in ion interception. The two-dimensional MXene membrane is applied to ion interception and is obtained by utilizing an electrophoretic deposition method. The application is specifically that a two-dimensional MXene membrane is placed in an ion interception device, an ionic compound solution is added into one side of the membrane, water is added into the other side of the membrane, and the two-dimensional MXene membrane realizes ion interception. The concentration of the ionic compound solution is 0.01-2 mol/L; the ionic compound is more than one of sodium chloride, lithium chloride, potassium chloride, magnesium chloride, aluminum chloride, copper chloride, sodium sulfate, lithium sulfate, potassium sulfate and aluminum sulfate. When the two-dimensional MXene film obtained by the electrophoretic deposition method is used for ion interception, the two-dimensional MXene film has a high interception effect on ions; and the membrane has good sealing performance, is not easy to fall off and is easy to assemble.
Description
Technical Field
The invention belongs to the field of preparation and ion interception of nano-membranes, and particularly relates to an application of a two-dimensional MXene membrane prepared by an electrophoretic deposition method in ion interception.
Background
Along with the shortage of global resources, the environment pollution situation is increasingly serious, and the shortage of fresh water resources is increasingly serious at present, so that the environmental problem becomes global. However, since nearly 97.5% of the total water resources in the world are salt water resources such as seawater and data shows that more than 70% of the population in the world live in a range of 70km from the seaside, desalination of seawater has been considered as the most practical method for continuously providing a fresh water source since the second half of the 20 th century.
Because the seawater has extremely high salt content and contains a large amount of microorganisms, the seawater can be drunk only by desalting. The core of seawater desalination lies in separating microorganisms and salt, in a physical method, heat energy is used as a driving force, and the method related to phase change in the brine separation process is classified into a thermal method which mainly comprises methods such as multi-stage flash evaporation, multi-effect distillation, vapor compression distillation, a freezing method, humidification and dehumidification and the like; brine separation using membranes (semipermeable membranes, ion exchange membranes, or the like) without involving phase change is classified into membrane methods, mainly including methods such as reverse osmosis and electrodialysis; traditional thermal separation methods such as rectification and the like have the advantages of complex operation, huge energy consumption and obvious membrane separation method advantages, can greatly reduce the energy consumption and improve the separation efficiency, and become the main trend of future development.
At present, the main methods for realizing large-scale industrialization are polymer films which have the defects of poor stability, no pollution resistance and the like. In recent years, with the rapid development of graphene oxide membranes in the field of ion separation, similar two-dimensional nano-membrane materials attract extensive attention of scientific research community due to the characteristics of good mechanical properties, high chemical stability, simple preparation, excellent performance and the like. Compared with a graphene oxide film, the two-dimensional transition metal carbonitride (MXene) film is simpler to prepare, higher in conductivity and better in hydrophilicity, and shows industrial application potential in the separation field, wherein the MXene material has a structural general formula of Mn+1XnOr (M1, M2)n+1XnOr Mn+1(X1,X2)nOne or a combination of two or more of them; said Mn+1XnWherein M ═ Ti, Nb, V, Mo, Zr, Cr, W, Ta; n is 1,2, 3; x ═ C, N; said (M)1,M2)n+1XnIn, M1,M2Ti, Nb, V, Mo, Zr, Cr, W, Ta; n is 1,2, 3; x ═ C, N; said Mn+1(X1,X2)nWherein M ═ Ti, Nb, V, Mo, Zr, Cr, W, Ta; n is 1,2, 3; x1,X2C, N. Present MXene film newspaperIn water treatment, most of the existing two-dimensional material MXene is applied to molecules or ions with larger particle sizes, but the trapping of small ions, namely reverse osmosis, is blank, so that the application of the MXene membrane to ion trapping has a great potential.
Disclosure of Invention
In order to improve the defects of the prior art and realize the breakthrough of the MXene membrane in the field of ion interception, the invention aims to provide the application of the two-dimensional MXene membrane prepared by an electrophoretic deposition method in the ion interception.
The purpose of the invention is realized by the following technical scheme:
the application of a two-dimensional MXene membrane in ion interception; the two-dimensional MXene film is obtained by an electrophoretic deposition method.
The two-dimensional MXene film is obtained by the following steps:
(1) etching MAX powder under the action of hydrochloric acid and lithium fluoride, centrifuging, washing, and ultrasonically dispersing to obtain MXene nanosheet solution;
(2) and carrying out electrophoretic deposition on the MXene nanosheet solution, and drying to obtain the two-dimensional MXene film.
The conditions of the electrophoretic deposition in the step (2): the voltage is 3-30V, and the time is 1-20 min. Or the current is 2-20 mA.
In the step (1), the mass-to-volume ratio of the lithium fluoride to the hydrochloric acid is (5-10) g: (100-200) mL;
the concentration of the hydrochloric acid solution is 6-12 mol/L.
In the step (1), the MAX powder is Ti2AlC、V2AlC、Ti3SiC2、Ti3AlC2、Ti4AlN3And Nb4AlC3One of (1); the mass ratio of the MAX powder to the lithium fluoride is (5-10): (5-10).
The etching time in the step (1) is 24-48 hours.
The solvent of the MXene nanosheet solution in the step (1) is water, and the concentration of the MXene nanosheet solution is 0.25-3 mg/ml.
The preparation method of the MXene nanosheet solution in the step (1) specifically comprises the following steps:
(a) adding villiaumite into a hydrochloric acid solution, uniformly stirring, adding MAX powder, stirring for reaction, centrifuging, washing and drying to obtain MXene powder;
(b) and dispersing MXene powder into a solvent, performing ultrasonic treatment and centrifugation, and taking an upper layer solution to obtain the MXene nanosheet solution.
The rotation speed of the stirring in the step (a) is 350 rpm; the rotation speed of the centrifuge is 2500 rpm; the time for centrifugation was 10 min. The washing in the step (a) is washing with deionized water until the pH is neutral (6-8).
The drying condition in the step (a) is that the temperature of forced air drying is 50-200 ℃; the drying time is 12-24 hours.
The ultrasonic time in the step (b) is 0.5-5 hours. The centrifugal rotating speed in the step (b) is 2000-3000 rpm; the centrifugation time is 1-3 hours.
The application of the two-dimensional MXene membrane in ion retention comprises the following steps:
and (2) placing the two-dimensional MXene membrane in an ion interception device, adding an ionic compound solution into one side of the membrane, adding water into the other side of the membrane, and realizing ion interception by the two-dimensional MXene membrane.
The concentration of the ionic compound solution is 0.01-2 mol/L, preferably 0.1-0.2 mol/L.
The ionic compound is sodium chloride, lithium chloride, potassium chloride, magnesium chloride, aluminum chloride, copper chloride, sodium sulfate, lithium sulfate, potassium sulfate, aluminum sulfate and the like. Wherein the two-dimensional MXene film has better interception effect on aluminum salt and copper metal salt.
The water is ultrapure water or deionized water.
The two-dimensional MXene film has no surface defects and good flexibility.
The two-dimensional MXene membrane prepared by the electrophoretic deposition method has higher ion interception performance and great application value in industry.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) when the two-dimensional MXene film prepared by the electrophoretic deposition method is used for ion interception, the two-dimensional MXene film has a high interception effect on ions.
(2) When the two-dimensional MXene membrane is used for ion interception, the sealing performance is good, the membrane is not easy to fall off, and the assembly is easy.
(3) The two-dimensional MXene membrane prepared by the electrophoretic deposition method is used for ion interception, has stable performance and good repeatability and has industrial application potential.
Drawings
FIG. 1 is a graph of permeation test of 0.2mol/L KCl solution in application example 1 of the present invention, with the ordinate being the conductivity of the solution on the permeation side and the abscissa being time;
FIG. 2 shows the results of example 2 of the present invention on 0.2mol/L AlCl3And (3) a solution permeation test chart, wherein the ordinate is the conductivity of the solution on the permeation side, and the abscissa is time.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The initial conductivity on the pure water side does not exceed 1.5 uS/cm. The conductivity meter of the conductivity measuring instrument is thunder magnetic DDSJ-31L.
Example 1
The application of the two-dimensional MXene membrane prepared by the electrophoretic deposition method in ion interception comprises the following steps:
(1) lithium fluoride (5g) was added to a hydrochloric acid solution (6mol/L, 100mL), stirred well, and 5g of MAX powder (Ti) was added3AlC2) Stirring at 350rpm for 24h, centrifuging at 2500rpm for 10min, washing with deionized water to pH 6, and drying at 60 deg.C for 12h to obtain Ti3C2TxMXene powder;
(2) mixing Ti3C2TxDispersing the powder into water, performing ultrasonic treatment for 2h, centrifuging, and taking an upper layer solution, namely an MXene nanosheet solution with the concentration of 2 mg/mL;
(3) taking Ti3C2TxThe MXene solution is put into a container, a positive electrode conductive porous substrate and a negative electrode conductive porous substrate are inserted, electrophoresis deposition is carried out by electrifying, the constant voltage is 30V, the time is 5min, then the substrate is taken out and dried in vacuum,obtaining a two-dimensional MXene film;
(4) taking the dried membrane off the substrate, or directly putting the membrane in a U-shaped groove with the substrate in between for fixation, adding the raw material liquid into one side of the membrane, adding ultrapure water into the other side of the membrane, adding stirrers into the two sides of the membrane for stirring, measuring the change of the conductivity of the pure water solution along with the time, and obtaining the permeation quantities of different ions through conversion.
In this example, when the raw material solution was a 0.2M sodium chloride solution, the permeation rate was 3.33X 10-3mol/m2H is used as the reference value. Permeation rate compared to substrate is 1mol/m2The reaction time per hour is obvious.
Example 2
The application of the two-dimensional MXene membrane prepared by the electrophoretic deposition method in ion interception comprises the following steps:
(1) lithium fluoride (10g) was added to a hydrochloric acid solution (12mol/L, 200mL), stirred well, and 10g of MAX powder (Ti) was added3AlC2) Stirring at 350rpm for 24h, centrifuging at 2500rpm for 10min, washing with deionized water to pH 6, and drying at 60 deg.C for 12h to obtain Ti2CTxMXene powder;
(2) mixing Ti3C2TxDispersing the powder into water, performing ultrasonic treatment for 1h, centrifuging, and taking an upper layer solution, namely an MXene nanosheet solution with the concentration of 3 mg/mL;
(3) taking Ti3C2TxAnd (3) placing the MXene solution in a container, inserting a positive electrode conductive substrate and a negative electrode conductive substrate with holes, electrifying for electrophoretic deposition, keeping the current at 14mA for 1min, taking out the substrates, and drying in vacuum.
Taking the dried film off the substrate, or directly putting the film in a U-shaped groove with the substrate in between for fixation, adding the raw material liquid into one side, adding ultrapure water into the other side, adding stirrers into the two sides for stirring, measuring the change of the conductivity of the pure water solution along with the time, and obtaining the permeation quantities of different ions through conversion.
In this example, when the raw material solution was a 0.2M sodium chloride solution, the permeation rate was 1.3X 10-2mol/m2H is used as the reference value. Permeation rate compared to substrate is 1mol/m2Has obvious interception actionThe application is as follows.
Example 3
The application of the two-dimensional MXene membrane prepared by the electrophoretic deposition method in ion interception comprises the following steps:
(1) lithium fluoride (8g) was added to a hydrochloric acid solution (6mol/L, 100mL), stirred well, and 5g of MAX powder (Ti) was added3AlC2) Stirring at 350rpm for 24h, centrifuging at 2500rpm for 10min, washing with deionized water to pH 6, and drying at 60 deg.C for 12h to obtain Ti3C2TxMXene powder;
(2) mixing Ti3C2TxDispersing the powder into water, performing ultrasonic treatment for 2h, centrifuging, and taking an upper layer solution, namely an MXene nanosheet solution with the concentration of 0.5 mg/mL;
(3) taking Ti3C2TxAnd (3) placing the MXene solution in a container, inserting a positive electrode conductive porous substrate and a negative electrode conductive porous substrate, electrifying for electrophoretic deposition at a constant voltage of 10V for 10min, and taking out the substrate and vacuum-drying the film.
Taking the dried film off the substrate, or directly putting the film in a U-shaped groove with the substrate in between for fixation, adding the raw material liquid into one side, adding ultrapure water into the other side, adding stirrers into the two sides for stirring, measuring the change of the conductivity of the pure water solution along with the time, and obtaining the permeation quantities of different ions through conversion.
When the raw material solution was a 0.2M sodium chloride solution, the permeation rate was 3.2X 10-2mol/m2H is used as the reference value. Permeation rate compared to substrate is 1mol/m2The reaction time per hour is obvious.
Application example 1
The application of the two-dimensional MXene membrane prepared by the electrophoretic deposition method in the ion interception is as follows:
the two-dimensional MXene membrane prepared by electrophoretic deposition in example 1 is fixed in the middle channel of an ion transmission testing U-shaped groove device by a gasket, and 50mL of 0.2mol/L KCl solution is added into the raw material side; 50mL of ultrapure water is added to the permeation side, a stirrer is added to the two sides for stirring, the rotation speed is 250rpm, and the conductivity change of water on the permeation side is detected by using a conductivity meter at room temperature. After 4h detection, the film was found to have a molar ratio to potassium chloride ionsThe average transmission rate is 3 x 10-3mol/m2The water flux was 0.12 g/bar/h. And even after the test for more than 6h, the permeation curve keeps a linear relation, which shows that the membrane has good stability in the permeation process. From the result, the MXene membrane with good ion retention performance can be quickly obtained by using the electrophoretic deposition preparation method, and the method has industrial application value. FIG. 1 is a graph showing permeation test of 0.2mol/L KCl solution in application example 1 of the present invention, with the ordinate representing the conductivity of the solution on the permeation side and the abscissa representing time.
Application example 2
The application of the two-dimensional MXene membrane prepared by the electrophoretic deposition method in the ion interception is as follows:
a two-dimensional MXene film prepared by electrophoretic deposition as described in example 1 was fixed in the middle channel of an ion transmission measuring U-tank apparatus by means of a gasket, and 0.2mol/L AlCl was added to the starting material side3100mL of the solution; 100mL of ultrapure water is added to the permeation side, a stirrer is added to the two sides for stirring, the rotation speed is 250rpm, and the conductivity change of water on the permeation side is detected by using a conductivity meter at room temperature. After 4h detection, the molar transmission rate of the membrane to aluminum chloride ions is found to be 2.41 multiplied by 10 on average-3mol/m2The water flux was 0.02 g/bar/h. And even after the test for more than 6h, the permeation curve keeps a linear relation, which shows that the membrane has good stability in the permeation process. From the result, the MXene membrane with good ion retention performance can be quickly obtained by using the electrophoretic deposition preparation method, and the method has industrial application value.
FIG. 2 shows the results of example 2 of the present invention on 0.2mol/L AlCl3And (3) a solution permeation test chart, wherein the ordinate is the conductivity of the solution on the permeation side, and the abscissa is time. The conductance of conventional tap water varies from a few hundred microsiemens per centimeter to thousands.
Claims (4)
1. The application of a two-dimensional MXene membrane in ion interception is characterized in that: the two-dimensional MXene film is obtained by an electrophoretic deposition method, and specifically, MXene nanosheet solution is subjected to electrophoretic deposition;
the two-dimensional MXene film is obtained by the following steps:
(1) adding 5g of lithium fluoride into 100mL of 6mol/L hydrochloric acid solution, stirring uniformly, adding 5g of Ti3AlC2Stirring the powder at 350rpm for 24h, centrifuging at 2500rpm for 10min, washing with deionized water until pH is 6, and drying at 60 deg.C for 12h to obtain Ti3C2TxMXene powder;
(2) mixing Ti3C2TxDispersing the powder into water, performing ultrasonic treatment for 2h, centrifuging, and taking an upper layer solution, namely an MXene nanosheet solution with the concentration of 2 mg/mL;
(3) taking Ti3C2TxAnd (3) putting the MXene solution into a container, inserting a positive electrode conductive porous substrate and a negative electrode conductive porous substrate, electrifying for electrophoretic deposition, keeping the constant voltage at 30V for 5min, taking out the substrates, and drying in vacuum to obtain the two-dimensional MXene film.
2. Use according to claim 1, characterized in that: the method comprises the following steps: and (2) placing the two-dimensional MXene membrane in an ion interception device, adding an ionic compound solution into one side of the membrane, adding water into the other side of the membrane, and realizing ion interception by the two-dimensional MXene membrane.
3. Use according to claim 2, characterized in that: the concentration of the ionic compound solution is 0.01-2 mol/L; the ionic compound is more than one of sodium chloride, lithium chloride, potassium chloride, magnesium chloride, aluminum chloride, copper chloride, sodium sulfate, lithium sulfate, potassium sulfate and aluminum sulfate.
4. Use according to claim 3, characterized in that: the ionic compound is more than one of aluminum chloride, copper chloride and aluminum sulfate.
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| CN112670365A (en) * | 2020-12-21 | 2021-04-16 | 华南理工大学 | GaAs/MXene heterojunction solar cell and preparation method thereof |
| CN112808018A (en) * | 2020-12-23 | 2021-05-18 | 华南理工大学 | Two-dimensional film continuous production process and equipment based on electrophoresis strategy |
| CN114592197B (en) * | 2022-01-20 | 2024-01-12 | 华南理工大学 | Two-dimensional g-C 3 N 4 Nanosheet film, electrochemical preparation method thereof and application of nanosheet film in ion separation |
| CN115812973B (en) * | 2022-12-13 | 2024-01-26 | 杭州佰倍优生物科技有限公司 | High-concentration albumin peptide beverage with good palatability |
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