CN113213598A - Ti-MXene derived sodium titanium phosphate/graphene composite material and preparation method and application thereof - Google Patents
Ti-MXene derived sodium titanium phosphate/graphene composite material and preparation method and application thereof Download PDFInfo
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- CN113213598A CN113213598A CN202110394430.6A CN202110394430A CN113213598A CN 113213598 A CN113213598 A CN 113213598A CN 202110394430 A CN202110394430 A CN 202110394430A CN 113213598 A CN113213598 A CN 113213598A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4691—Capacitive deionisation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
Abstract
The invention discloses a Ti-MXene derived sodium titanium phosphate/graphene composite material and a preparation method and application thereof. The method is based on the principle that Faraday capacitance and double electric layer capacitance store charges. In a capacitance deionization device, under the condition of a certain voltage, Ti-MXene derived titanium sodium phosphate/graphene composite material is taken as a Faraday capacitor to adsorb sodium ions, and active carbon is taken as an electric double layer to adsorb chloride ions in a capacitance deionization device, so that sodium chloride is removed, and the aim of desalting is fulfilled. The cyclic adsorption and desorption of the material to chloride ions and sodium ions can be realized by controlling the magnitude of the applied voltage and adjusting the positive and negative electrodes, the operation is simple, no secondary pollution is caused, and the assistance of other chemical substances is not needed. The adsorption capacity of a hybrid capacitive deionization device composed of a Ti-MXene derived sodium titanium phosphate/graphene composite material and an activated carbon electrode on sodium chloride can reach 251.55mg g‑1And has lower energy consumption of 0.19 kWh.kg-NaCl‑1Is a promising desalting method.
Description
Technical Field
The invention belongs to the technical field of high-energy electrochemistry, and relates to preparation of a Ti-MXene derived sodium titanium phosphate/graphene electrode material and application of the Ti-MXene derived sodium titanium phosphate/graphene electrode material in a hybrid capacitance deionization technology.
Background
With the rapid increase of the world population and the gradual increase of the environmental pollution, people face a severe drinking water safety crisis. In addition, China also faces more and more serious problem of water resource shortage. According to related data, the per-capitalized fresh water possession of China is only 2200 cubic meters, which is famous for 121 in the world and is less than one third of the per-capitalized water resource in the world, and belongs to one of 13 countries with the most shortage of the per-capitalized water resource in the world. However, the water consumption of China maintains a higher level for a long time, and the water pollution increases the brackish water ratio, so that the problem of severe water resource shortage of China is caused.
Aiming at the problem of shortage of drinking water resources, the most common method at present is to purify bitter water or seawater which can not be directly cited, thereby relieving the crisis of shortage of fresh water resources.
The traditional capacitive deionization technology is that external voltage is applied to two ends of a porous carbon-based electrode, so that negative and positive ions move to the electrode with opposite electric properties under the action of an electrostatic field, and are adsorbed on the electrode, and water resources are recycled through short circuit or reverse connection of a power supply. However, conventional carbon-based electrodes tend to undergo electrode oxidation due to long-term cycling, and the adsorption capacity is affected by the specific surface area of the material, and the charge efficiency is affected by the co-ion efficiency, so that a new electrode material is needed for desalination.
Disclosure of Invention
The invention aims to overcome the defects of the traditional capacitance deionization technology and the electrode material on the basis of the traditional capacitance deionization technology, and provides a preparation method of a Ti-MXene derived titanium sodium phosphate/graphene composite material and application of the Ti-MXene derived titanium sodium phosphate/graphene composite material in a hybrid capacitance deionization technology.
Firstly, preparing a Ti-MXene derived sodium titanium phosphate/graphene composite material, wherein the electrode material is subjected to sodium removal and sodium insertion through Faraday reaction under the action of voltage, and is less influenced by an electrode compared with a traditional carbon electrode; and secondly, compared with the traditional capacitance deionization technology, the application of the hybrid capacitance deionization technology has higher adsorption capacity, namely, external voltage is applied to two ends of a porous electrode, so that negative and positive ions move to the electrode with opposite electric property under the action of an electrostatic field, and are adsorbed on the electrode, and the regeneration and utilization are carried out by reversely connecting a power supply. Compared with the traditional carbon electrode, the Ti-MXene derived sodium titanium phosphate/graphene composite material system is subjected to sodium intercalation and sodium desorption through faradaic reaction, and has a good electrochemical window, a large specific capacitance and good stability, so that the Ti-MXene derived sodium titanium phosphate/graphene composite material system has a good application prospect in the field of capacitive deionization.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
1. firstly, the method for preparing the Ti-MXene derived sodium titanium phosphate/graphene composite material comprises the following steps:
(1) mixing Ti3C2TxAnd graphene according to a mass ratio of 4: 1 mixing to form a stable solution A;
(2) respectively adding 200ul of hydrogen peroxide, 2ml of phosphoric acid and 100mg of sodium acetate into the solution A under the condition of stirring, and stirring to obtain a solution B;
(3) transferring the solution B to a hydrothermal kettle, heating for 5 hours at 160 ℃, washing the obtained product with deionized water and ethanol, and drying in a vacuum drying oven;
(4) and (4) annealing the dried sample at 700 ℃ for 4h under the argon atmosphere.
Preparation of Ti-MXene derived sodium titanium phosphate/graphene composite material and application of the Ti-MXene derived sodium titanium phosphate/graphene composite material in capacitive deionization technology.
The Ti-MXene derived sodium titanium phosphate/graphene composite material prepared by the preparation method.
The particle size of the Ti-MXene derived sodium titanium phosphate/graphene composite material is micron-sized.
An application of Ti-MXene derived sodium titanium phosphate/graphene composite material in a hybrid capacitance deionization technology is as follows:
firstly, preparing a Ti-MXene derived sodium titanium phosphate/graphene composite material and an activated carbon electrode:
(1) grinding the prepared Ti-MXene derived sodium titanium phosphate/graphene composite material, and then mixing the ground Ti-MXene derived sodium titanium phosphate/graphene composite material with the mass ratio of 8: 1: 1, PVDF and acetylene black are mixed and stirred for about 6 to 12 hours to obtain evenly mixed slurry, the slurry is coated on a graphite paper collector and dried at the temperature of 60 ℃ in vacuum to obtain a Ti-MXene derived sodium titanium phosphate/graphene electrode;
(2) the preparation method of the activated carbon electrode is similar to that of the activated carbon electrode, and the Ti-MXene derived titanium sodium phosphate/graphene composite material is replaced by activated carbon.
Next, assembly of the hybrid capacitive deionization apparatus:
(3) the hybrid capacitor deionization device is formed by sequentially assembling a fixing plate, a silica gel gasket, a collector electrode, a Ti-MXene derived sodium titanium phosphate/graphene electrode, an organic glass water collecting tank, a diaphragm, an anion exchange membrane, an activated carbon electrode, the collector electrode, the silica gel gasket and the fixing plate. Wherein, the organic glass water collecting tank is a hollow plate and is provided with a water inlet and a water outlet, thereby achieving the purpose of circulating water inlet.
Finally, desalting performance test:
(4) and after the hybrid capacitor deionization device is assembled, the hybrid capacitor deionization device is connected into a desalination process to be subjected to desalination performance test. The desalting process comprises a sodium chloride collecting tank, a peristaltic pump, a hybrid capacitance deionization device and a conductivity meter, wherein all the devices are connected through hoses. When the device works, the peristaltic pump inputs sodium chloride brine from the sodium chloride collecting tank into the electrified hybrid capacitance deionization device at a certain speed, and the sodium chloride brine is circulated back to the sodium chloride collecting tank to test the conductivity of the solution after adsorption.
(5) The desorption process can be realized by reverse connection of voltage, and the operation is consistent with the adsorption.
The principle of removing sodium chloride ions in water by the hybrid capacitance deionization technology is as follows: under the condition of external voltage, sodium ions in crystal lattices of the Ti-MXene derived titanium sodium phosphate/graphene composite material are removed, and the sodium ions in the solution can be re-embedded into the crystal lattices by reverse voltage connection, so that the sodium ions in the water body are removed; the chloride ions move to the activated carbon electrode under the action of external voltage, an electric double layer is formed on the surface of the activated carbon electrode and stored, and when the voltage is reversely connected, the electric double layer disappears and the chloride ions are desorbed from the electrode; therefore, the process of cyclic regeneration of material adsorption and desorption is achieved.
The anion exchange membrane is used for reducing the effect of co-ions in the reaction process, thereby increasing the charge efficiency.
The flow rate of circulating water of the peristaltic pump is 20 ml/min.
The cyclic regeneration conditions are as follows: the voltage range is-1.8V to-1.0V; the constant current density range is 30 mA/g-100 mA/g.
The inlet water concentration is as follows: the concentration of inlet water is 1000 mg/L.
The traditional capacitive deionization technology utilizes a carbon-based electrode, removes ions by forming a double electric layer, and has the defects of small adsorption capacity and the like. Compared with the electric double layer behavior, the cell behavior (namely bulk phase faradaic reaction) has larger specific capacitance, which indicates that the cell has larger adsorption capacity when being applied to the field of capacitive deionization. In the invention, a hybrid capacitance deionization technology is utilized, one pole of the hybrid capacitance deionization technology generates a Faraday reaction, and the other pole of the hybrid capacitance deionization technology is still a carbon-based electrode; meanwhile, the double advantages of double electric layer behaviors and battery behaviors are combined, so that larger adsorption capacity can be obtained, and the adsorption rate can be ensured.
Compared with the prior art, the invention has the beneficial effects that: firstly, the invention removes the sodium chloride in the water body based on the Faraday capacitance and the double electric layer capacitance, and can achieve the recycling. The invention has large adsorption capacity, high adsorption rate and low energy consumption.
Drawings
Fig. 1 is a TEM image of a Ti-MXene-derived sodium titanium phosphate/graphene composite material provided in example 1 of the present invention.
Fig. 2 is an SEM image of the Ti-MXene-derived sodium titanium phosphate/graphene composite material provided in embodiment 1 of the present invention.
Fig. 3 is a schematic diagram of a hybrid capacitive deionization electrode provided in embodiment 2 of the present invention.
Fig. 4 is a schematic diagram of a process for deriving Ti-MXene from sodium titanium phosphate/graphene according to embodiment 2 of the present invention.
FIG. 5 is a graph of the adsorption capacity of hybrid capacitor for deionization at different concentrations as provided in example 2 of the present invention.
FIG. 6 is a graph of the adsorption capacity and adsorption rate of hybrid capacitor deionization under different voltage windows as provided in example 2 of the present invention.
FIG. 7 shows the energy consumption and charge efficiency of hybrid capacitor deionization at different voltages according to example 2 of the present invention.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1
Preparing a Ti-MXene derived sodium titanium phosphate/graphene composite material:
(1) mixing Ti3C2TxAnd graphene in a mass ratio of 4: 1 mixing to form a stable solution A; (ii) a
(2) Respectively adding 200ul of hydrogen peroxide, 2ml of phosphoric acid and 100mg of sodium acetate into the solution A under the condition of stirring, and stirring to obtain a solution B;
(3) transferring the solution B to a hydrothermal kettle, heating for 5 hours at 160 ℃, washing the obtained product with deionized water and ethanol, and drying in a vacuum drying oven;
(4) and (4) annealing the dried sample at 700 ℃ for 4h under the argon atmosphere.
The resulting Ti-MXene-derived sodium titanium phosphate graphene composite material, used to provide example 2 for further application testing, is shown in TEM and SEM images in fig. 1 and 2: graphene platelets and MXene residual platelets can be observed, with the square size of sodium titanium phosphate being about 500nm to 1 μm. And ordered composition of graphene/MXene and derived titanium sodium phosphate can be seen.
Example 2
Application of Ti-MXene derived sodium titanium phosphate/graphene composite material in hybrid capacitance deionization technology.
Preparing a Ti-MXene derived sodium titanium phosphate/graphene composite material electrode and an activated carbon electrode:
and (3) mixing the prepared Ti-MXene derived sodium titanium phosphate/graphene composite material and activated carbon according to the mass ratio of 8: 1: 1, PVDF and acetylene black are mixed, NMP is added, the mixture is stirred for about 6 hours to obtain evenly mixed slurry, the slurry is coated on a graphite paper collector, and the Ti-MXene derived sodium titanium phosphate/graphene composite material electrode and an activated carbon electrode can be obtained by drying the slurry at the temperature of 60 ℃ in vacuum.
Testing the desalting performance:
using 1000mg L-1Rinsing the hybrid capacitor deionization device with a sodium chloride solution, adding 50mL of the sodium chloride solution into the test solution tank, and continuously circulating until the conductivity is basically stable; on the basis of the above steps, applying a constant current to both ends of the electrode, starting desalination, and simultaneously recording the current and the change of the solution conductivity, wherein the current is recorded every 5s, and the conductivity is recorded every 10 s; and when the conductivity of the solution reaches basic stability, the experimental adsorption is finished. Adsorbing byThe process schematic diagram is shown in fig. 3, sodium ions move to the Ti-MXene derived titanium sodium phosphate/graphene composite material electrode under the action of an electric field, and chloride ions move to the activated carbon electrode. And (5) changing the direction of a power supply to perform desorption, and exporting data through a computer after the experiment is completed. Fig. 4 shows the change process of sodium ions in the phase lattice of the material in the adsorption and desorption processes. The adsorption performance is shown in fig. 5, 6 and 7:
FIG. 5 shows the desalination performance of different initial sodium chloride concentrations in a capacitive deionization system comprising Ti-MXene-derived sodium titanium phosphate/graphene as an anode and activated carbon as a cathode. As the concentration increases, the desalting capacity increases, the initial sodium chloride concentration is 20mM, the operation voltage is 1.8V, and the maximum adsorption capacity can be 278.03 mg/g.
FIG. 6 shows the desalination performance of the capacitive deionization system composed of Ti-MXene derived sodium titanium phosphate/graphene as the anode and activated carbon as the cathode under different operating voltages. With the increase of the operating voltage, the adsorption capacity is continuously increased, and the adsorption rate changes correspondingly and continuously decrease. When the operating voltage reaches 1.8V, the adsorption capacity can reach 263mg/g, and the rate is 0.027 mg/g/s.
Fig. 7 shows the charge efficiency and energy consumption changes under different operating voltage conditions of the capacitive deionization system composed of Ti-MXene derived sodium titanium phosphate/graphene as the anode and activated carbon as the cathode. The charge efficiency drops slightly with increasing voltage, but a relatively high charge efficiency (greater than 80%) is maintained. And the energy consumption is gradually increased along with the increase of the voltage, and the energy consumption is minimum 0.19kWh/kg when the operating voltage is 1.0V.
Compared with the traditional carbon-based capacitor, the deionization adsorption capacity and the charge efficiency are greatly improved, the energy consumption is reduced, and the method has wider application prospect.
The above description is only illustrative of the preferred embodiments of the present invention and should not be taken as limiting the scope of the invention in any way. Any changes or modifications made by those skilled in the art based on the above disclosure should be considered as equivalent effective embodiments, and all the changes or modifications should fall within the protection scope of the technical solution of the present invention.
Claims (8)
1. A preparation method of Ti-MXene derived sodium titanium phosphate/graphene composite material is characterized in that,
the method comprises the following steps:
firstly, preparing a Ti-MXene derived sodium titanium phosphate/graphene composite material:
(1) mixing Ti3C2TxAnd graphene according to a mass ratio of 4: 1 mixing to form a stable solution A;
(2) respectively adding 200ul of hydrogen peroxide, 2ml of phosphoric acid and 100mg of sodium acetate into the solution A under the condition of stirring, and stirring to obtain a solution B;
(3) transferring the solution B to a hydrothermal kettle, heating for 5 hours at 160 ℃, washing the obtained product with deionized water and ethanol, and drying in a vacuum drying oven;
(4) and (4) annealing the dried sample for 2h at 700 ℃ in an argon atmosphere.
2. The Ti-MXene derived sodium titanium phosphate/graphene composite material obtained by the preparation method of claim 1.
3. The Ti-MXene-derived sodium titanium phosphate/graphene composite material of claim 2, wherein: the particle size of the Ti-MXene derived sodium titanium phosphate/graphene composite material is micron-sized.
4. The application of the Ti-MXene derived sodium titanium phosphate/graphene composite material in the hybrid capacitance deionization technology is characterized by comprising the following steps:
preparing a Ti-MXene derived sodium titanium phosphate/graphene composite material electrode and an activated carbon electrode:
(1) grinding the prepared Ti-MXene derived sodium titanium phosphate/graphene composite material, and then mixing the ground Ti-MXene derived sodium titanium phosphate/graphene composite material with the following components in a mass ratio of 8: 1: 1, PVDF and acetylene black, adding a proper amount of NMP, stirring for about 6-12 hours to obtain uniformly mixed slurry, and smearing the slurry on a graphite paper collector. Drying at 60 ℃ in vacuum to obtain a Ti-MXene derived sodium titanium phosphate/graphene composite material electrode;
(2) the method comprises the following steps of (1) mixing activated carbon according to a mass ratio of 8: 1:: 1, PVDF and acetylene black are mixed and stirred for about 6 to 12 hours to obtain evenly mixed slurry, the slurry is coated on a graphite paper collector and dried at the temperature of 60 ℃ in vacuum to obtain an activated carbon electrode;
assembling the capacitive deionization device:
(3) the desalting performance test is carried out by sequentially assembling a fixed plate, a silica gel gasket, a collector, a Ti-MXene derived sodium titanium phosphate/graphene electrode, an organic glass water collecting tank, a diaphragm, an anion exchange membrane, an activated carbon electrode, the collector, the silica gel gasket and the fixed plate in the device. Wherein, the organic glass water collecting tank is a hollow plate and is provided with a water inlet and a water outlet, thereby achieving the purpose of circulating water inlet;
testing the desalting performance:
(4) after the hybrid capacitor deionization device is assembled, the hybrid capacitor deionization device is connected into a desalination process, the desalination process is executed by adopting a sodium chloride collecting tank, a peristaltic pump, the hybrid capacitor deionization device and a conductivity meter, and all devices are connected through hoses; when the device works, the peristaltic pump inputs sodium chloride brine from the sodium chloride collecting tank into the electrified hybrid capacitance deionization device at a certain speed, and the sodium chloride brine is circulated back to the sodium chloride collecting tank to test the conductivity meter after adsorption;
(5) the desorption process can be realized by reversely connecting a power supply, and the operation is consistent with the adsorption.
5. Use according to claim 4, characterized in that: the flow rate of circulating water of the peristaltic pump is 20 ml/min.
6. Use according to claim 4, characterized in that: the influent concentration during the desalting performance test was 1000 mg/L.
7. Use according to claim 4, characterized in that: the cyclic regeneration conditions during the desalting performance test were: the voltage range is-1.8V to-1.0V; the constant current density range is 30 mA/g-100 mA/g.
8. Use according to claim 4, characterized in that: in the desalination performance test process, when adsorbing, connecting the Ti-MXene derived sodium titanium phosphate/graphene composite material with a negative electrode to adsorb sodium ions, and connecting an active carbon electrode with a positive electrode to adsorb chloride ions; the desorption can be achieved by connecting the voltage reversely.
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