CN113912063A - Ti3C2TxBase electrode material and preparation method and application thereof - Google Patents
Ti3C2TxBase electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a Ti3C2T x The preparation method comprises the following steps: (1) mixing Ti3C2T x Diluting after ultrasonic centrifugation; (2) mixing Ti3C2T x Placing the multi-walled carbon nanotube (MWNT) and the MWNT in a beaker, diluting, ultrasonically stirring, adding concentrated hydrochloric acid, and uniformly shaking; (3) pouring a mixed solution of carbon tetrachloride and aniline; (4) adding ammonium persulfate into the mixed solution, fully reacting, centrifuging, washing with water, and freeze-drying to obtain Ti3C2T x MWNT/PANI powder; (5) ti3C2T x dispersing/MWNT/PANI powder in ethanol, adding carbon black and PTFE, coating on a substrate, and drying to obtain Ti3C2T x An MWNT/PANI based electrode material. The electrode material prepared by the invention has large specific surface area and high adsorption capacity up to 258 mg.g‑1，Ti3C2T x Provides an ion transport channel and shortens an ion transport path, realizes high capacity and high speed, has a simple preparation method, and is Ti3C2T x Provides a prospect in the field of seawater desalination.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to Ti3C2TxA base electrode material, a preparation method and application thereof.
Background
Fresh water resources on the earth are insufficient and unevenly distributed, and population faces extreme water shortage crisis. The full utilization of seawater resources is one of effective ways for solving the problem of insufficient water supply at present, and the exploration of a green and environment-friendly treatment way becomes a hot topic. The technologies of reverse osmosis, electrodialysis and the like occupy the mainstream of the market, but all the technologies need high power consumption and operation cost, or are large-scale infrastructures and are easy to scale. Capacitive Deionization (CDI) is considered to be the most promising method for providing fresh water to human beings as a novel technology with low consumption, high efficiency, low cost and no secondary pollution. However, the conventional CDI system has problems of low deionization capacity, poor cycle stability, low electric adsorption capacity, etc., which seriously hinders its practical application.
Research aiming at electrode materials can effectively improve the performance of CDI devices, and various carbon materials and composite carbon electrode materials are sequentially applied to the field of capacitive desalination. Drewes et al treated NaCl solutions with carbon aerogel as the electrode material to an adsorption capacity of 7.0mg/g at a voltage of 1.3V (Xu Pei et al, Water Research,2008,42(10-11), 2605-2617). The activated carbon fiber electrode prepared by Qiujieshan et al has an electric adsorption capacity of 4.46mg/g at 1.6V (Wang Gang et al, Electrochimica Acta,2012,69, 65-70). The carbon material has the advantages of high available specific surface area, multidimensional holes, good conductivity, high specific capacitance, excellent electrochemical stability and the like, and can effectively improve the adsorption capacity and adsorption and desorption efficiency of capacitive deionization.
MXene is Gogotsi and Barsodium, and a novel transition metal carbide and nitrogen are discovered in 2011The two-dimensional material of the compound stores charges through ion embedding between two-dimensional layered structures and presents ideal pseudocapacitance. Wherein, Ti3C2TxIs one of the most common MXene materials at present, and due to the graphene-like layered structure, the huge specific surface area and the abundant active sites, the MXene materials provide ion transport channels and shorten ion transport paths. In addition, the material has the advantages of hydrophilicity, ion conductivity, excellent conductivity and the like, and is a promising capacitive deionization electrode material. Pattarachai Srimuk followed by Mohammad Tokamanzadeh et al utilized Ti3C2TxThe prepared electrode material has the adsorption capacity of 12-13mg/g (Srimuk Patcaracai et al, J.Mater.chem.A., 2016,4 (47)), 18265-&Tokamanzadeh Mohammad et al, ACS appl. Mater. interfaces,2020,12(23), 26013-. But Ti3C2TxThe lamella is easy to stack, the transport path of ions between layers is long, the regulation direction of the microstructure of the ion is limited, and the adsorption capacity and the adsorption and desorption rate of the ion are poor.
Disclosure of Invention
Aiming at the prior art Ti3C2TxThe invention aims to provide Ti with large adsorption capacity and high adsorption rate3C2TxA base electrode material. The electrode material prepared by the invention has larger specific surface area, Ti3C2TxIons are adsorbed between the sheets to form a network structure with MWNT, a channel is provided for solution immersion and ion diffusion, the adsorption rate is effectively improved, the adsorption capacity is increased, and the introduction of PANI enables the particles to have higher specific capacitance of Ti3C2TxProvides better prospect in the field of seawater desalination.
In order to achieve the purpose, the invention adopts the following technical scheme:
ti3C2TxThe preparation method of the base electrode material comprises the following steps:
(1) ti to be prepared3C2TxDispersingLiquid ultrasonic treatment, centrifugation, sediment removal, supernatant dilution to obtain Ti3C2TxDispersing the solution;
(2) adding Ti obtained in the step (1)3C2TxAdding MWNT into the dispersion solution, adding water for dilution, performing ultrasonic treatment, and stirring to obtain Ti3C2TxThe MWNT compound dispersion liquid is added with concentrated hydrochloric acid;
(3) pouring carbon tetrachloride and aniline monomers into a beaker, and uniformly mixing;
(4) mixing the solutions obtained in the step (2) and the step (3), adding an ammonium persulfate aqueous solution, and fully reacting to obtain Ti3C2Txa/MWNT/PANI complex dispersion;
(5) ti obtained in the step (4)3C2Txcentrifuging/MWNT/PANI compound dispersion liquid, washing with water, and freeze-drying to obtain Ti3C2TxMWNT/PANI powder;
(6) dispersing the powder obtained in the step (5) in ethanol, adding carbon black and PTFE, performing ultrasonic treatment, coating on a substrate, and drying to obtain Ti3C2TxAn MWNT/PANI based electrode material.
Preferably, said Ti in step (1)3C2TxThe preparation method of the dispersion comprises the following steps: injecting 15mL of 12MHCl into a 50mL test tube, and adding 1g of LiF for dissolution to obtain an etching solution; then, 1g of Ti3AlC2Adding into the prepared solution, shaking, placing the test tube in a 60 deg.C water bath kettle for reaction for 72h, centrifuging with deionized water, washing, and centrifuging to obtain Ti3C2TxPowder of Ti3C2TxDispersing the powder in water to obtain the Ti3C2TxAnd (3) dispersing the mixture.
Preferably, said Ti in step (1)3C2TxThe dispersion liquid is subjected to ultrasonic treatment for 3-4 h in 300-400W cell disruption, the centrifugation is carried out for 25-35min at 3000-3500r/min, and Ti is added3C2TxThe concentration of the dispersion was 5 mg/ml-1。
Preferably, Ti in step (2)3C2TxThe mass ratio of the MWNT powder to the MWNT powder is 1:9-9:1, the volume of the MWNT powder after being diluted by water is 20ml, the ultrasonic treatment is carried out for 10-20min under 400-500W, the stirring is carried out for 4-5h under 400-600r/min, and the adding amount of concentrated hydrochloric acid is 1 ml.
Preferably, in step (3), 90-100ml of carbon tetrachloride and 1ml of aniline monomer are mixed uniformly.
Preferably, the ammonium persulfate aqueous solution in the step (4) is prepared by weighing 0.276g of ammonium persulfate and adding 1.5-2ml of deionized water; the reaction is carried out for 10-12h at 20-30 ℃.
Preferably, the complex dispersion liquid in the step (5) is centrifuged for 15-20min at 7000-8000r/min, washed for 3-4 times and freeze-dried for 36-48 h.
Preferably, the substrate in the step (6) is graphite paper, and 50mg of Ti is weighed3C2TxDispersing the/MWNT/PANI powder in 1-2ml ethanol, adding 6-6.5mg carbon black and 4-4.1 μ l PTFE, performing ultrasonic treatment at 300W and 400W for 10-15min, and drying in a vacuum drying oven at 60 ℃ for 24 h.
The invention also claims Ti prepared by the preparation method3C2TxBase electrode material and said Ti3C2TxUse of a base electrode material for capacitive deionization.
Compared with the prior art, the invention has the following beneficial effects:
the invention is to etch Ti3AlC2Ti prepared by ultrasonic method3C2TxThe graphene-like layered structure is beneficial to enlarging the storable space of ions so as to improve the adsorption capacity of the ions. During the preparation process, the Ti sheets are mixed mechanically3C2TxThe MWNT is compounded with the MWNT, utilizes the one-dimensional structure of the multi-walled carbon nano-tube to increase the specific surface area of the multi-walled carbon nano-tube, is inserted into the MWNT in the nano-sheet layer, can play a role in connecting each sheet layer, and is connected with Ti3C2TxAnd a network structure is formed, so that the transportation of electrons is promoted, and the adsorption rate is improved. Then in-situ polymerizing to obtain the product with large ratioPANI of the capacitor is firmly connected with Ti3C2TxThe combination of MWNT effectively increases the adsorption capacity of the material, and finally the composite electrode material with excellent capacitive deionization performance is obtained. Further, MWNT and Ti3C2TxAnd PANI forms a network structure, so that the transmission rate of electrons between layers and the absorption and desorption rate of ions are improved.
Drawings
FIG. 1 is Ti prepared in example 33C2TxXPS plot of/MWNT/PANI; (a) full spectrum (b) N1 s (C) Ti 2p (d) C1 s;
FIG. 2 is Ti prepared in example 33C2TxSEM image of/MWNT/PANI;
FIG. 3 is a schematic diagram of the CDI performance testing process of the present invention.
Detailed Description
The present invention will be described in more detail with reference to specific preferred embodiments, but the present invention is not limited to the following embodiments.
It should be noted that, unless otherwise specified, the chemical reagents involved in the present invention are commercially available.
In this example, Ti3AlC2Particles less than 40 microns, available from Beijing Lianli New Technology co.
Example 1
Ti3C2TxThe preparation method of the base electrode material is characterized by comprising the following steps of:
(1)Ti3C2Txpreparation of the dispersion: injecting 15mL of 12M HCl into a 50mL test tube, and adding 1g of LiF for dissolving to obtain an etching solution; then, 1g of Ti3AlC2Adding into the prepared solution, shaking, placing the test tube in a 60 deg.C water bath for reaction for 72h, centrifuging and washing with deionized water for three times after the reaction is finished, and centrifuging at 5000rpm for 5min to obtain Ti3C2TxPowder of Ti3C2TxDispersing the powder in water to obtain the Ti3C2TxAnd (3) dispersing the mixture.
(2) Ti prepared in the step (1)3C2TxSubjecting the dispersion to ultrasonic treatment in 300W cell disruptor for 3h, centrifuging at 3500r/min for 30min, removing precipitate, and diluting the supernatant to 5mg mL-1To obtain Ti3C2TxDispersing the solution;
(3) adding 0.8ml of Ti obtained in the step (2)3C2TxAdding 36mgMWNT into the dispersion solution, diluting with water to 20ml, performing 400W ultrasonic treatment for 15min, stirring at 500r/min for 4h to obtain Ti3C2TxThe MWNT compound dispersion liquid is added with 1ml of concentrated hydrochloric acid;
(4) pouring 100ml of carbon tetrachloride and 1ml of aniline monomer into a beaker, and uniformly mixing;
(5) weighing 0.276mg of ammonium persulfate, adding 1.5ml of deionized water, and uniformly shaking;
(6) mixing the solutions obtained in the steps (3) and (4), adding the ammonium persulfate aqueous solution obtained in the step (5), and reacting at 25 ℃ for 10h to obtain Ti3C2Txa/MWNT/PANI complex dispersion;
(7) ti obtained in the step (6)3C2TxCentrifuging at 8000r/min for 15min, washing with water for 3 times, and freeze drying for 48 hr to obtain Ti3C2TxMWNT/PANI powder;
(8) dispersing 50mg of the powder obtained in the step (7) in 1.5ml of ethanol, adding 6.25mg of carbon black and 4.1 mu l of PTFE, performing 400W ultrasonic treatment for 10min, coating the mixture on a graphite paper substrate, drying the graphite paper substrate in a vacuum drying oven at 60 ℃ for 24h, and drying to obtain Ti3C2TxAn MWNT/PANI based electrode material.
Example 2
Ti3C2TxThe preparation method of the base electrode material is characterized by comprising the following steps of:
(1)Ti3C2Txpreparation of the dispersion: injecting 15mL of 12M HCl into a 50mL test tube, and adding 1g of LiF for dissolving to obtain an etching solution; then, 1g of Ti3AlC2Adding into the above prepared solution, and shakingPlacing the test tube in a 60 ℃ water bath kettle for reaction for 72 hours, after the reaction is finished, centrifugally washing the test tube for three times by deionized water, and centrifuging the test tube at 5000rpm for 5 minutes to obtain Ti3C2TxPowder of Ti3C2TxDispersing the powder in water to obtain the Ti3C2TxAnd (3) dispersing the mixture.
(2) Ti prepared in the step (1)3C2TxSubjecting the dispersion to ultrasonic treatment in 300W cell disruptor for 3h, centrifuging at 3500r/min for 30min, removing precipitate, and diluting the supernatant to 5mg mL-1To obtain Ti3C2TxDispersing the solution;
(3) adding 2.4ml of Ti obtained in the step (2)3C2TxAdding 28mgMWNT into the dispersion solution, diluting with water to 20ml, performing 400W ultrasonic treatment for 15min, stirring at 500r/min for 4h to obtain Ti3C2TxThe MWNT compound dispersion liquid is added with 1ml of concentrated hydrochloric acid;
(4) pouring 100ml of carbon tetrachloride and 1ml of aniline monomer into a beaker, and uniformly mixing;
(5) weighing 0.276mg of ammonium persulfate, adding 1.5ml of deionized water, and uniformly shaking;
(6) mixing the solutions obtained in the steps (3) and (4), adding the ammonium persulfate aqueous solution obtained in the step (5), and reacting at 25 ℃ for 10h to obtain Ti3C2Txa/MWNT/PANI complex dispersion;
(7) ti obtained in the step (6)3C2TxCentrifuging at 8000r/min for 15min, washing with water for 3 times, and freeze drying for 48 hr to obtain Ti3C2TxMWNT/PANI powder;
(8) dispersing 50mg of the powder obtained in the step (7) in 1.5ml of ethanol, adding 6.25mg of carbon black and 4.1 mu l of PTFE, performing 400W ultrasonic treatment for 10min, coating the mixture on a graphite paper substrate, drying the graphite paper substrate in a vacuum drying oven at 60 ℃ for 24h, and drying to obtain Ti3C2TxAn MWNT/PANI based electrode material.
The sample prepared in this example was used for capacitive deionization performance studies.
According to the table1, at 2000 mg.L for NaCl solutions of different concentrations-1When the adsorption capacity of the material reaches the maximum value of 210mg g-1The adsorption rate is 1000 mg.L-1The highest value is reached.
Example 3
Ti3C2TxThe preparation method of the base electrode material is characterized by comprising the following steps of:
(1)Ti3C2Txpreparation of the dispersion: injecting 15mL of 12M HCl into a 50mL test tube, and adding 1g of LiF for dissolving to obtain an etching solution; then, 1g of Ti3AlC2Adding into the prepared solution, shaking, placing the test tube in a 60 deg.C water bath for reaction for 72h, centrifuging and washing with deionized water for three times after the reaction is finished, and centrifuging at 5000rpm for 5min to obtain Ti3C2TxPowder of Ti3C2TxDispersing the powder in water to obtain the Ti3C2TxAnd (3) dispersing the mixture.
(2) Ti prepared in the step (1)3C2TxSubjecting the dispersion to ultrasonic treatment in 300W cell disruptor for 3h, centrifuging at 3500r/min for 30min, removing precipitate, and diluting the supernatant to 5mg mL-1To obtain Ti3C2TxDispersing the solution;
(3) adding 4ml of Ti obtained in the step (2)3C2TxAdding 20mgMWNT into the dispersion solution, diluting with water to 20ml, performing 400W ultrasonic treatment for 15min, stirring at 500r/min for 4h to obtain Ti3C2TxThe MWNT compound dispersion liquid is added with 1ml of concentrated hydrochloric acid;
(4) pouring 100ml of carbon tetrachloride and 1ml of aniline monomer into a beaker, and uniformly mixing;
(5) weighing 0.276mg of ammonium persulfate, adding 1.5ml of deionized water, and uniformly shaking;
(6) mixing the solutions obtained in the steps (3) and (4), adding the ammonium persulfate aqueous solution obtained in the step (5), and reacting at 25 ℃ for 10h to obtain Ti3C2Txa/MWNT/PANI complex dispersion;
(7) ti obtained in the step (6)3C2TxCentrifuging at 8000r/min for 15min, washing with water for 3 times, and freeze drying for 48 hr to obtain Ti3C2TxMWNT/PANI powder;
(8) dispersing 50mg of the powder obtained in the step (7) in 1.5ml of ethanol, adding 6.25mg of carbon black and 4.1 mu l of PTFE, performing 400W ultrasonic treatment for 10min, coating the mixture on a graphite paper substrate, drying the graphite paper substrate in a vacuum drying oven at 60 ℃ for 24h, and drying to obtain Ti3C2TxAn MWNT/PANI based electrode material.
And analyzing and observing the taken sample through a scanning electron microscope, X-ray photoelectron spectroscopy and the like, and using the sample for the research on the capacitive deionization performance.
According to FIGS. 1 and 2, Ti3C2TxThe MWNT and the PANI are successfully compounded together, and the MWNT is at Ti3C2The surface of the T and the interlayer form an interlayer network, and the function of promoting electron transportation is achieved. According to Table 1, the concentration of NaCl solution was 2000 mg.L-1When the adsorption capacity and the adsorption rate of the material reach the maximum value, the adsorption capacity and the adsorption rate of the material are respectively 258mg g-1And 8.6mg g-1·min-1Compared with the data measured in example 2, the electrode material prepared in example 3 has a larger adsorption capacity and a two-fold higher adsorption rate due to the fact that the MWNT contained in example 3 is higher in proportion, more electron transport bridges are constructed between layers, and the specific surface area is larger.
Example 4
Ti3C2TxThe preparation method of the base electrode material is characterized by comprising the following steps of:
(1)Ti3C2Txpreparation of the dispersion: injecting 15mL of 12M HCl into a 50mL test tube, and adding 1g of LiF for dissolving to obtain an etching solution; then, 1g of Ti3AlC2Adding into the prepared solution, shaking, placing the test tube in a 60 deg.C water bath for reaction for 72h, centrifuging and washing with deionized water for three times after the reaction is finished, and centrifuging at 5000rpm for 5min to obtain Ti3C2TxPowder of and thenTi3C2TxDispersing the powder in water to obtain the Ti3C2TxAnd (3) dispersing the mixture.
(2) Ti prepared in the step (1)3C2TxSubjecting the dispersion to ultrasonic treatment in 300W cell disruptor for 3h, centrifuging at 3500r/min for 30min, removing precipitate, and diluting the supernatant to 5mg mL-1To obtain Ti3C2TxDispersing the solution;
(3) adding 5.6ml of Ti obtained in the step (2)3C2TxAdding 12mgMWNT into the dispersion solution, diluting with water to 20ml, performing 400W ultrasonic treatment for 15min, stirring at 500r/min for 4h to obtain Ti3C2TxThe MWNT compound dispersion liquid is added with 1ml of concentrated hydrochloric acid;
(4) pouring 100ml of carbon tetrachloride and 1ml of aniline monomer into a beaker, and uniformly mixing;
(5) weighing 0.276mg of ammonium persulfate, adding 1.5ml of deionized water, and uniformly shaking;
(6) mixing the solutions obtained in the steps (3) and (4), adding the ammonium persulfate aqueous solution obtained in the step (5), and reacting at 25 ℃ for 10h to obtain Ti3C2Txa/MWNT/PANI complex dispersion;
(7) ti obtained in the step (6)3C2TxCentrifuging at 8000r/min for 15min, washing with water for 3 times, and freeze drying for 48 hr to obtain Ti3C2TxMWNT/PANI powder;
(8) dispersing 50mg of the powder obtained in the step (7) in 1.5ml of ethanol, adding 6.25mg of carbon black and 4.1 mu l of PTFE, performing 400W ultrasonic treatment for 10min, coating the mixture on a graphite paper substrate, drying the graphite paper substrate in a vacuum drying oven at 60 ℃ for 24h, and drying to obtain Ti3C2TxAn MWNT/PANI based electrode material.
Example 5
Ti3C2TxThe preparation method of the base electrode material is characterized by comprising the following steps of:
(1)Ti3C2Txpreparation of the dispersion: 15mL of 12M HCl was injected into 50mLAdding 1g of LiF into a test tube for dissolution to obtain an etching solution; then, 1g of Ti3AlC2Adding into the prepared solution, shaking, placing the test tube in a 60 deg.C water bath for reaction for 72h, centrifuging and washing with deionized water for three times after the reaction is finished, and centrifuging at 5000rpm for 5min to obtain Ti3C2TxPowder of Ti3C2TxDispersing the powder in water to obtain the Ti3C2TxAnd (3) dispersing the mixture.
(2) Ti prepared in the step (1)3C2TxSubjecting the dispersion to ultrasonic treatment in 300W cell disruptor for 3h, centrifuging at 3500r/min for 30min, removing precipitate, and diluting the supernatant to 5mg mL-1To obtain Ti3C2TxDispersing the solution;
(3) adding 7.2ml of Ti obtained in the step (2)3C2TxAdding 4mgMWNT into the dispersion solution, diluting with water to 20ml, performing 400W ultrasonic treatment for 15min, stirring at 500r/min for 4h to obtain Ti3C2TxThe MWNT compound dispersion liquid is added with 1ml of concentrated hydrochloric acid;
(4) pouring 100ml of carbon tetrachloride and 1ml of aniline monomer into a beaker, and uniformly mixing;
(5) weighing 0.276mg of ammonium persulfate, adding 1.5ml of deionized water, and uniformly shaking;
(6) mixing the solutions obtained in the steps (3) and (4), adding the ammonium persulfate aqueous solution obtained in the step (5), and reacting at 25 ℃ for 10h to obtain Ti3C2Txa/MWNT/PANI complex dispersion;
(7) ti obtained in the step (6)3C2TxCentrifuging at 8000r/min for 15min, washing with water for 3 times, and freeze drying for 48 hr to obtain Ti3C2TxMWNT/PANI powder;
(8) dispersing 50mg of the powder obtained in the step (7) in 1.5ml of ethanol, adding 6.25mg of carbon black and 4.1 mu l of PTFE, performing 400W ultrasonic treatment for 10min, coating the mixture on a graphite paper substrate, drying the graphite paper substrate in a vacuum drying oven at 60 ℃ for 24h, and drying to obtain Ti3C2TxAn MWNT/PANI based electrode material.
Comparative example 1
Ti3C2TxThe preparation method of the base electrode material is characterized by comprising the following steps of:
(1)Ti3C2Txpreparation of the dispersion: injecting 15mL of 12M HCl into a 50mL test tube, and adding 1g of LiF for dissolving to obtain an etching solution; then, 1g of Ti3AlC2Adding into the prepared solution, shaking, placing the test tube in a 60 deg.C water bath for reaction for 72h, centrifuging and washing with deionized water for three times after the reaction is finished, and centrifuging at 5000rpm for 5min to obtain Ti3C2TxPowder of Ti3C2TxDispersing the powder in water to obtain the Ti3C2TxAnd (3) dispersing the mixture.
(2) Ti prepared in the step (1)3C2TxSubjecting the dispersion to ultrasonic treatment in 300W cell disruptor for 3h, centrifuging at 3500r/min for 30min, removing precipitate, and collecting supernatant to obtain Ti3C2TxDispersing the solution;
(3) ti obtained in the step (2)3C2TxThe dispersion is frozen and dried for 48 hours to obtain Ti3C2TxPowder;
(4) dispersing 50mg of the powder obtained in the step (3) in 1.5ml of ethanol, adding 6.25mg of carbon black and 4.1 mu l of PTFE, performing 400W ultrasonic treatment for 10min, coating the mixture on a graphite paper substrate, drying the graphite paper substrate in a vacuum drying oven at 60 ℃ for 24h, and drying to obtain Ti3C2TxA base electrode material.
The samples prepared in examples 2 to 3 and comparative example 1 were used for capacitive deionization performance studies. CDI performance test method:
(1) weighing the mass of the graphite paper before coating, and obtaining the mass of the electrode material after fluorine coating and drying;
(2) configuration of 100-3000 mg/ml-1200ml of NaCl solution;
(3) the samples prepared in examples 2 to 3 and comparative example 1 were used as negative electrodes, and an activated carbon electrode was used as a positive electrode, and the devices were connected as shown in fig. 3;
(4) an electrochemical workstation is used for providing a voltage of 1.2V;
(5) opening the peristaltic pump, starting to operate the conductivity meter after water is discharged, and operating the electrochemical workstation;
(6) the solution concentration is obtained by a conductivity meter, and the adsorption capacity and the adsorption rate of the material are calculated according to the following formula:
TABLE 1 data table of capacitive deionization performance test of electrode materials prepared in examples 2 to 3 and comparative example 1
According to Table 1, pure Ti3C2TxThe adsorption capacity of the base electrode material is only 18mg g-1The adsorption rate is only 1mg g-1·min-1And is to be promoted.
Finally, it is to be noted that: the above examples do not limit the invention in any way. It will be apparent to those skilled in the art that various modifications and improvements can be made to the present invention. Accordingly, any modification or improvement made without departing from the spirit of the present invention is within the scope of the claimed invention.
Claims (10)
1. Ti3C2TxThe preparation method of the base electrode material is characterized by comprising the following steps of:
(1) ti to be prepared3C2TxUltrasonic treatment of the dispersion, centrifugation, removal of precipitate, and dilution of the supernatant to obtain Ti3C2TxDispersing the solution;
(2) adding Ti obtained in the step (1)3C2TxAdding MWNT into the dispersion solution, adding water for dilution, performing ultrasonic treatment, and stirring to obtain Ti3C2TxThe MWNT compound dispersion liquid is added with concentrated hydrochloric acid;
(3) pouring carbon tetrachloride and aniline monomers into a beaker, and uniformly mixing;
(4) mixing the solutions obtained in the step (2) and the step (3), adding an ammonium persulfate aqueous solution, and fully reacting to obtain Ti3C2Txa/MWNT/PANI complex dispersion;
(5) ti obtained in the step (4)3C2Txcentrifuging/MWNT/PANI compound dispersion liquid, washing with water, and freeze-drying to obtain Ti3C2TxMWNT/PANI powder;
(6) dispersing the powder obtained in the step (5) in ethanol, adding carbon black and PTFE, performing ultrasonic treatment, coating on a substrate, and drying to obtain Ti3C2TxAn MWNT/PANI based electrode material.
2. The Ti of claim 13C2TxThe method for preparing the base electrode material is characterized in that the Ti in the step (1)3C2TxThe preparation method of the dispersion comprises the following steps: injecting 15mL of 12M HCl into a 50mL test tube, and adding 1g of LiF for dissolving to obtain an etching solution; then, 1g of Ti3AlC2Adding into the prepared solution, shaking, placing the test tube in a 60 deg.C water bath kettle for reaction for 72h, centrifuging with deionized water, washing, and centrifuging to obtain Ti3C2TxPowder of Ti3C2TxDispersing the powder in water to obtain the Ti3C2TxAnd (3) dispersing the mixture.
3. The Ti of claim 13C2TxThe method for preparing the base electrode material is characterized in that the Ti in the step (1)3C2TxThe dispersion liquid is subjected to ultrasonic treatment for 3-4 h in 300-400W cell disruption, the centrifugation is carried out for 25-35min at 3000-3500r/min, and Ti is added3C2TxThe concentration of the dispersion was 5 mg/ml-1。
4. The Ti of claim 13C2TxThe preparation method of the base electrode material is characterized in that Ti in the step (2)3C2TxThe mass ratio of the MWNT powder to the MWNT powder is 1:9-9:1, the volume of the MWNT powder after being diluted by water is 20ml, the ultrasonic treatment is carried out for 10-20min under 400-500W, the stirring is carried out for 4-5h under 400-600r/min, and the adding amount of concentrated hydrochloric acid is 1 ml.
5. The Ti of claim 13C2TxThe preparation method of the base electrode material is characterized in that 90-100ml of carbon tetrachloride and 1ml of aniline monomer are uniformly mixed in the step (3).
6. The Ti of claim 13C2TxThe preparation method of the base electrode material is characterized in that the ammonium persulfate aqueous solution in the step (4) is prepared by weighing 0.276g of ammonium persulfate and adding 1.5-2ml of deionized water; the reaction is carried out for 10-12h at 20-30 ℃.
7. The Ti of claim 13C2TxThe preparation method of the base electrode material is characterized in that the compound dispersion liquid in the step (5) is centrifuged for 15-20min at 7000-8000r/min, washed for 3-4 times and freeze-dried for 36-48 h.
8. The Ti of claim 13C2TxThe preparation method of the base electrode material is characterized in that the substrate in the step (6) is graphite paper, and 50mg of Ti is weighed3C2TxMWNT/PANI powderDispersing in 1-2ml ethanol, adding 6-6.5mg carbon black and 4-4.1 μ l PTFE, ultrasonic treating at 300-400W for 10-15min, and drying in vacuum drying oven at 60 deg.C for 24 h.
9. Ti prepared by the preparation method of any one of claims 1 to 83C2TxA base electrode material.
10. A Ti as set forth in claim 93C2TxUse of a base electrode material for capacitive deionization.
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| CN115074086A (en) * | 2022-07-14 | 2022-09-20 | 西北工业大学 | Zn-MOFs derived ZnO/C/Ti 3 C 2 Composite wave-absorbing material and preparation method thereof |
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