CN114700095A - One-dimensional CdS nanorod/three-dimensional multilayer Ti3C2Preparation method of composite photocatalyst - Google Patents
One-dimensional CdS nanorod/three-dimensional multilayer Ti3C2Preparation method of composite photocatalyst Download PDFInfo
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- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 65
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
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Abstract
The invention discloses a one-dimensional CdS nanorod/three-dimensional multilayer Ti3C2The preparation method of the composite photocatalyst comprises the following steps: (1) mixing Ti3AlC2Adding the powder into a hydrofluoric acid solution, and reacting for 20-28 hours at constant temperature under magnetic stirring; (2) repeatedly washing the obtained material until the pH value is 7; (3) preparation of multilayer Ti3C2Powder; (4) preparation of Cd2+/Ti3C2Mixing the solution; (5) dissolving thiourea in an ethylenediamine solution, uniformly mixing to obtain thiourea/ethylenediamine, and adding the thiourea/ethylenediamine into the Cd prepared in the step (5)2+/Ti3C2Uniformly mixing the mixed solution; (6) pouring the mixed solution prepared in the step (5) into a reactor for hydrothermal reaction, and then sequentially cooling and separatingWashing and vacuum drying to obtain CdS/Ti3C2A catalyst. The invention prepares three-dimensional multilayer Ti by a chemical etching method3C2The CdS nano-rod grows in situ and is loaded on the three-dimensional multilayer Ti by utilizing a hydrothermal solvent self-assembly synthesis method3C2To obtain the one-dimensional CdS nanorod/three-dimensional multilayer Ti3C2The preparation method of the composite photocatalyst has the advantages of simple operation, high quality and good repeatability.
Description
Technical Field
The invention belongs to the technical field of photocatalyst preparation, and particularly relates to a one-dimensional CdS nanorod/three-dimensional multilayer Ti3C2A preparation method of a composite photocatalyst.
Background
The development of clean energy has attracted attention in recent years in order to control pollution, protect environment and realize sustainable development, and hydrogen production by decomposing water through photocatalysis is a promising method for relieving energy and environmental crisis.
Since Graphene (Graphene) was successfully prepared in 2004, two-dimensional layered materials became one of the research hotspots of material science. In 2011, a novel two-dimensional transition group metal carbon/nitrogen compound, namely MXenes material, is successfully prepared and is gradually applied to the fields of lithium ion batteries, supercapacitors, catalysis and the like in recent years. MXenes is a new family of two-dimensional transition metal carbides synthesized by selective exfoliation of ternary carbides, nitrides or carbonitrides of general formula Mn+1XnWherein M represents a transition metal (e.g., Sc, Ti, Ta, Cr, Mo, etc.), and X is C and/or N. Density Functional Theory (DFT) calculations indicate that MXenes exhibit metallic conductivity and have been explored for use in catalysis, energy storage and conversion, among other fields. It has also been shown in experimental characterization to be key to achieving effective catalysis in Hydrogen Evolution Reactions (HER), suggesting that MXenes may be photocatalytic H2Good cocatalyst of (2).
The surface of the MXene material is provided with a large number of hydrophilic functional groups (-OH, -O and-F), and the functional groups can enable the MXene material to be firmly connected with a plurality of semiconductor materials; in addition, MXenes materials have excellent metal conductivity, and can ensure efficient carrier migration on the surface thereof. The excellent characteristics make MXenes material as cocatalyst possess great application potential in photocatalysis field.
Thus, two-dimensional graphene-based layered materials are considered to be the most promising candidates for various catalytic applications. Ti3C2As one of the most commonly used members of the MXenes family, there are advantages of large numbers of bare metal atoms, ultra-thin two-dimensional layered structure, highly hydrophilic surface, excellent light absorption properties and good electrical conductivity. Studies have shown that Ti will have high conductivity3C2The catalyst is used as a cocatalyst, so that an efficient heterojunction can be constructed, the carrier mobility is enhanced, and the catalytic performance is improved.
The CdS used as the main photocatalytic material has some defects, and the defects limit the further application development of the CdS. For example, CdS is susceptible to photo-corrosion and thus to loss of reactivity. In addition, the easy aggregation of CdS nanoparticles is limiting H2Another disadvantage of the yield. This is because the agglomeration of catalyst particles inevitably leads to a decrease in the effective catalytic specific surface area and accelerates the polymerization of photogenerated electrons-holes generated during the photocatalytic process, greatly reducing the catalytic activity. In order to overcome the above defects, many methods for improving the photocatalytic activity of CdS have been proposed, including forming a complex of CdS of quantum dots and other compounds, doping ions, and the like. The hydrogen production experiment and the photoelectric test result of the patent show that the CdS nano-particles and the multilayer Ti with good conductivity are used3C2The composite heterojunction can effectively improve the separation rate of electron-hole pairs and improve the catalytic activity of the catalyst; and the close combination mode effectively avoids the photo-corrosion of the CdS nano particles, thereby improving the stability of the catalyst.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a one-dimensional CdS nanorod/three-dimensional multilayer Ti3C2Preparation method of composite photocatalyst, and preparation of three-dimensional multilayer Ti by chemical etching method3C2The CdS nano-rod grows in situ and is loaded on the three-dimensional multilayer Ti by utilizing a hydrothermal solvent self-assembly synthesis method3C2To obtain the one-dimensional CdS nanorod/three-dimensional multilayer Ti3C2A composite photocatalyst is provided.
In order to achieve the above purpose, one of the technical solutions of the present invention is: one-dimensional CdS nanorod/three-dimensional multilayer Ti3C2The preparation method of the composite photocatalyst comprises the following steps of3AlC2Preparing three-dimensional multilayer Ti by a chemical etching method as a raw material3C2(ii) a By utilizing a hydrothermal solvent self-assembly synthesis method, the CdS nano-rod grows in situ and is loaded on the three-dimensional multilayer Ti3C2To obtain the one-dimensional CdS nanorod/three-dimensional multilayer Ti3C2A composite photocatalyst is provided.
The preparation method specifically comprises the following steps:
(1) placing hydrofluoric acid in a reactor, placing the reactor on a magnetic stirrer, and weighing a certain amount of Ti3AlC2Adding the powder into a hydrofluoric acid solution, and reacting for 20-28h at constant temperature;
(2) repeatedly washing the material obtained in the step (1) until the pH value of the collected washing liquid is 7 to remove the residual hydrofluoric acid and Al3+Ions;
(3) vacuum drying the material obtained in the step (2) for 20-28h, and grinding the dried sample to obtain multilayer Ti3C2；
(4) Taking Ti prepared in the step (3) in a certain mass3C2Powder, evenly dispersing the powder in a certain volume of ethylenediamine solution to obtain Ti3C2Extracting cadmium nitrate (Cd (NO) from ethylenediamine solution3)2.4H2O) is dissolved in ethylenediamine solution with certain volume to obtain cadmium nitrate/ethylenediamine solution, and the cadmium nitrate/ethylenediamine solution and the ethylenediamine solution are mixed uniformly to obtain Cd2+/Ti3C2Mixing the solution;
(5) dissolving thiourea in an ethylenediamine solution, uniformly mixing to obtain thiourea/ethylenediamine, and adding the thiourea/ethylenediamine into the Cd prepared in the step (5)2+/Ti3C2Mixing the solution evenly;
(6) pouring the mixed solution prepared in the step (5) into a reactor for hydrothermal reaction, and then sequentially cooling, centrifugally washing and vacuum drying to obtain CdS/Ti3C2A catalyst.
In a preferred embodiment of the present invention, the hydrofluoric acid solution in the step (1) has a mass fraction of 40%, and the hydrofluoric acid solution is mixed with Ti3AlC2The volume-mass ratio is 8-12 mL/g.
In a preferred embodiment of the present invention, the reactor in the step (1) is an uncovered polytetrafluoroethylene reaction kettle, Ti3AlC2The hydrofluoric acid solution is added slowly to avoid overheating of the reaction and Ti3AlC2Agglomerating, and keeping the constant temperature at 35-45 ℃.
In a preferred embodiment of the present invention, the material washing manner in the step (2) is repeated washing with water and alcohol alternately.
In a preferred embodiment of the present invention, the material drying temperature in the step (3) is 45 to 55 ℃.
In a preferred embodiment of the present invention, Ti in said step (4)3C2The mass volume ratio of the powder to the ethylenediamine solution is 0.3-3mg/mL, and the molar volume ratio of the cadmium nitrate to the ethylenediamine solution is 0.5-1 mmol/mL.
Still more preferably, Ti in said step (4)3C2The volume ratio of the solution of the ethylene diamine to the solution of the cadmium nitrate to the solution of the ethylene diamine is 2-4:1-3, and the mixing mode is that the solution of the cadmium nitrate to the solution of the ethylene diamine is slowly dripped into Ti3C2In the ethylene diamine solution, the mixture is evenly mixed by ultrasonic or stirring.
In a preferred embodiment of the invention, the molar volume ratio of the thiourea to the ethylenediamine in the step (5) is 1.8-2.1mmol/mL, the solution is added in a manner of slow pouring, Cd2+/Ti3C2The volume ratio of the ethylenediamine solution to the thiourea/ethylenediamine solution is 4-6:1-3, and the uniform mixing mode is stirring and mixing.
In a preferred embodiment of the present invention, the hydrothermal reaction temperature in the step (6) is 150 ℃ and 170 ℃, and the reaction time is 20-26 h.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention can be utilizedChemical etching method and hydrothermal solvent self-assembly method for preparing one-dimensional CdS nanorod/three-dimensional multilayer Ti3C2Composite photocatalyst, and strong acid etching to remove Ti3AlC2Middle Al3+Atom to produce three-dimensional Ti3C2Powder; adopting a hydrothermal solvent self-assembly method, and taking ethylenediamine as a hydrothermal solvent to enable the one-dimensional CdS nano-rod to grow on the three-dimensional multilayer Ti3C2The above step (1); in the process of stirring and mixing reactants, the ethylenediamine and the Cd2+Forming a complex, which is beneficial to forming a regular one-dimensional CdS nanorod; in the hydrothermal reaction process, the ethylenediamine provides alkaline reaction conditions and is used as a coupling agent for CdS and Ti3C2The heterojunction is formed by connecting the two layers together, so that the electron transmission capacity is effectively improved, and the carrier recombination rate is reduced;
2. the preparation method of the invention has simple operation, high quality and good repeatability, and compared with the prior art, the preparation method not only can prepare a large amount of novel high-efficiency one-dimensional CdS nano rods/three-dimensional multilayer Ti3C2The composite photocatalyst has the advantages of low operation difficulty, strong feasibility, short preparation period, low cost and the like.
Drawings
FIG. 1 is a three-dimensional multilayer Ti of example 1 of the present invention3C2X-ray diffraction pattern of (a).
FIG. 2 shows a one-dimensional CdS nanorod/three-dimensional multilayer Ti in example 1 of the present invention3C2X-ray diffraction pattern of the composite photocatalyst.
FIG. 3 shows a one-dimensional CdS nanorod/three-dimensional multilayer Ti in example 1 of the present invention3C2Scanning electron microscope photo of the composite photocatalyst.
FIG. 4 shows a one-dimensional CdS nanorod/three-dimensional multi-layer Ti in example 1 of the present invention3C2Scanning electron microscope energy spectrum photo of the composite photocatalyst.
FIG. 5 shows a one-dimensional CdS nanorod/three-dimensional multilayer Ti in example 1 of the present invention3C2And (5) a transmission electron microscope photo of the composite photocatalyst.
FIG. 6 shows a one-dimensional CdS nanorod/three-dimensional multi-layer Ti in example 1 of the present invention3C2And (3) an ultraviolet visible diffuse reflection absorbance spectrum of the composite photocatalyst.
FIG. 7 shows a one-dimensional CdS nanorod/three-dimensional multi-layer Ti in example 1 of the present invention3C2And the ultraviolet visible diffuse reflection band gap diagram of the composite photocatalyst.
FIG. 8 shows a one-dimensional CdS nanorod/three-dimensional multilayer Ti in example 1 of the present invention3C2The EIS Nyquist spectrum of the composite photocatalyst.
FIG. 9 shows a one-dimensional CdS nanorod/three-dimensional multi-layer Ti in example 1 of the present invention3C2And (3) a transient photocurrent response diagram of the composite photocatalyst.
FIG. 10 shows a one-dimensional CdS nanorod/three-dimensional multilayer Ti in example 1 of the present invention3C2And (3) a steady-state fluorescence spectrum of the composite photocatalyst.
FIG. 11 shows a one-dimensional CdS nanorod/three-dimensional multilayer Ti in example 1 of the present invention3C2And (4) comparing the hydrogen production of the composite photocatalyst.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in more detail below with reference to the accompanying drawings and specific embodiments, but the scope of the present invention is not limited to these embodiments.
One-dimensional CdS nanorod/three-dimensional multilayer Ti3C2The preparation method of the composite photocatalyst specifically comprises the following steps:
(1) placing hydrofluoric acid in a reactor, placing the reactor on a magnetic stirrer, and weighing a certain amount of Ti3AlC2Adding the powder into a hydrofluoric acid solution, and reacting for 20-28h at constant temperature;
(2) repeatedly washing the material obtained in the step (1) until the pH value of the collected washing liquid is 7 to remove the residual hydrofluoric acid and Al3+Ions;
(3) vacuum drying the material obtained in the step (2) for 20-28h, and grinding the dried sample to obtain multilayer Ti3C2Powder;
(4) taking a certain mass of the above Ti3C2Powder of, let itUniformly dispersing in a certain volume of ethylenediamine solution to obtain Ti3C2Extracting cadmium nitrate (Cd (NO) from ethylenediamine solution3)2.4H2O) is dissolved in a certain volume of ethylenediamine solution to obtain cadmium nitrate/ethylenediamine solution, and the cadmium nitrate/ethylenediamine solution is slowly dripped into Ti3C2Mixing the solution of ethylene diamine uniformly to obtain Cd2+/Ti3C2Mixing the solution;
(5) dissolving thiourea in an ethylenediamine solution, uniformly mixing to obtain thiourea/ethylenediamine, and adding the thiourea/ethylenediamine into the Cd prepared in the step (5)2+/Ti3C2Mixing the solution evenly;
(6) pouring the mixed solution prepared in the step (5) into a reactor for hydrothermal reaction, and then sequentially cooling, centrifugally washing and vacuum drying to obtain CdS/Ti3C2A catalyst.
The mass fraction of the hydrofluoric acid solution in the step (1) is 40%, and the hydrofluoric acid solution and Ti are3AlC2The volume-mass ratio is 8-12 mL/g.
The reactor in the step (1) is an uncovered polytetrafluoroethylene reaction kettle and Ti3AlC2The hydrofluoric acid solution is added slowly to avoid overheating of the reaction and Ti3AlC2Agglomerating, and keeping the constant temperature at 35-40 ℃.
And (3) the material washing mode in the step (2) is water and alcohol alternately and repeatedly washing.
The material drying temperature in the step (3) is 45-55 ℃.
Ti in the step (4)3C2The mass-volume ratio of the powder to the ethylenediamine solution is 0.3-3mg/mL, and the molar volume ratio of the cadmium nitrate to the ethylenediamine solution is 0.5-1 mmol/mL.
Ti in the step (4)3C2The volume ratio of the solution of the ethylene diamine to the solution of the cadmium nitrate to the solution of the ethylene diamine is 2-4:1-3, and the mixing mode is that the solution of the cadmium nitrate to the solution of the ethylene diamine is slowly dripped into Ti3C2In the ethylene diamine solution, the mixture is evenly mixed by ultrasonic or stirring.
In the step (5), the mol of thiourea and the ethylene diamine is adoptedThe volume ratio is 1.8-2.1mmol/mL, the solution is added in a mode of slow pouring, Cd2+/Ti3C2The volume ratio of the ethylenediamine solution to the thiourea/ethylenediamine solution is 4-6:1-3, and the uniform mixing mode is stirring and mixing.
The hydrothermal reaction temperature in the step (6) is 150-170 ℃, and the reaction time is 20-26 h.
Example 1
(1) Taking 20mL of hydrofluoric acid with the mass fraction of 40 wt% in a polytetrafluoroethylene cup, placing the hydrofluoric acid on a magnetic stirrer for stirring, and weighing 2g of Ti3AlC2Slowly adding the powder into a hydrofluoric acid solution for 10 minutes, and reacting for 24 hours at constant temperature under the stirring condition at 40 ℃;
(2) washing the material obtained in the step (1) with water and alcohol alternately and repeatedly until the pH of the washing liquid is 7 to remove residual hydrofluoric acid and Al3+Ions;
(3) vacuum drying the material obtained in the step (2) for 24 hours, and grinding the dried sample to obtain multilayer Ti3C2Powder;
(4) taking 50mg of Ti prepared in the step (3)3C2Adding the powder into 30mL of ethylenediamine solution, and performing ultrasonic treatment for 2 hours to uniformly disperse the powder; taking 15mmol of cadmium nitrate (Cd (NO))3.4H2O), adding the mixture into 20mL of ethylenediamine solution, and stirring to uniformly mix the mixture; pouring cadmium nitrate/ethylenediamine solution into Ti which is continuously stirred3C2Stirring in ethylenediamine solution at room temperature for 12 hr to obtain Cd2+/Ti3C2Mixing the solution;
(5) dissolving 45mmol of thiourea in 20mL of ethylenediamine solution, and stirring to mix uniformly; adding the thiourea/ethylenediamine solution into Cd2+/Ti3C2Mixing the solution, stirring for 3 hours to uniformly mix the solution to obtain a mixed solution;
(6) transferring the mixed solution obtained in the step (5) to a 100mL polytetrafluoroethylene high-pressure reaction kettle, and reacting for 2 days at 160 ℃; then sequentially cooling, centrifugally washing and vacuum drying to obtain CdS/Ti3C2A catalyst product.
The above multilayer Ti3C2The powder has X-ray diffraction pattern shown in FIG. 1, and characteristic peak of diffraction of Ti3C2A sharp peak indicates that the crystal has good crystallinity and purity; the corresponding transmission electron micrograph is shown in FIG. 5(b), and it can be seen that Ti is present3C2The multilayer sheet structure of (1).
Prepared CdS/Ti3C2The X-ray diffraction pattern of the catalyst is shown in figure 2, due to the combination with Ti3C2The intensity of the diffraction peak of the CdS is reduced relative to pure CdS powder; the scanning electron micrograph of the CdS/Ti is shown in FIG. 3(b) (FIG. 3(a) is the scanning electron micrograph of pure CdS), and the CdS/Ti is obtained by self-assembly of hydrothermal solvent3C2Catalyst, in which one-dimensional CdS nanorods are uniformly attached to and grown on three-dimensional Ti3C2Surface and interlayer; the scanning electron micrograph thereof is shown in FIG. 4, from which it can be seen that CdS/Ti are included3C2The catalyst comprises Cd element (figure 4(b)) and S element (figure 4(c)) which are uniformly distributed in the catalyst.
For CdS/Ti3C2The results of the transmission electron microscope observation of the catalyst are shown in FIG. 5, in which FIG. 5(a), FIG. 5(b), and FIG. 5(c) correspond to pure CdS and Ti, respectively3C2、CdS/Ti3C2The transmission electron microscope photo also proves that the one-dimensional CdS nano rod grows on the multilayer Ti3C2Surface and interlayer; the ultraviolet visible diffuse reflection absorbance spectrum is shown in FIG. 6, which shows CdS/Ti3C2The catalyst has better light absorption performance; the ultraviolet visible diffuse reflection band gap diagram is shown in FIG. 7, one-dimensional CdS and three-dimensional Ti3C2The composite effectively reduces the band gap of the CdS catalyst, and shows that one-dimensional CdS and three-dimensional Ti3C2The compound of (2) can improve the electron transmission capability and the photocatalysis performance; the EIS Nyquist diagram of the composite material is shown in FIG. 8, which shows that the composite material has smaller charge transfer resistance and is beneficial to the transmission and separation of carriers; the transient photocurrent response graph is shown in FIG. 9, the photocurrent density is increased to 5 times of CdS, which shows that the composite Ti is synthesized3C2Increased response to light, Ti3C2Facilitating more carrier generation and separation; the steady state fluorescence spectrum is shown in figure 10, and the improvement of the carrier separation effect is also proved.
The catalyst product prepared by the embodiment and pure CdS prepared by the same method are catalyzed to carry out photocatalytic performance test, lactic acid is used as a sacrificial agent and is uniformly mixed with water under the condition of simulating sunlight, the mixture is detected and evaluated in a water photolysis hydrogen production system, the photocatalytic hydrogen production map is shown in figure 11, and the compounded CdS/Ti3C2The photocatalytic hydrogen production performance of the catalyst is far higher than that of a pure CdS catalyst, and the hydrogen production rate is as high as 6.67 mmol/h-1·g-14 times that of the pure CdS sample; the catalyst product prepared in this example, one-dimensional CdS nanorod/three-dimensional multilayer Ti, is illustrated3C2The composite photocatalyst has excellent photocatalytic activity, can realize high-efficiency decomposition of water to produce hydrogen under sunlight, and is high-efficiency and energy-saving.
The above embodiments are merely preferred embodiments of the present invention, which are provided for illustrating the principles and effects of the present invention and not for limiting the present invention. It should be noted that modifications to the above-described embodiments can be made by persons skilled in the art without departing from the spirit and scope of the invention, and such modifications should also be considered as within the scope of the invention.
Claims (10)
1. One-dimensional CdS nanorod/three-dimensional multilayer Ti3C2The preparation method of the composite photocatalyst is characterized by comprising the following steps:
(1) taking hydrofluoric acid into a reactor, and then adding Ti3AlC2Reacting the powder for 20-28 hours under the magnetic stirring at constant temperature;
(2) washing the material obtained in the step (1) until the pH value of a washing liquid is neutral;
(3) vacuum drying the material obtained in the step (2) for 20-28h, and grinding to obtain multilayer Ti3C2Powder;
(4) taking the Ti prepared in the step (3)3C2Dispersing the powder in an ethylenediamine solution to obtain Ti3C2Dissolving cadmium nitrate in ethylenediamine solution to obtain nitric acidCadmium/ethylenediamine solution, and then the cadmium/ethylenediamine solution and the ethylenediamine solution are mixed uniformly to obtain Cd2+/Ti3C2Mixing the solution;
(5) dissolving thiourea in an ethylenediamine solution to obtain a thiourea/ethylenediamine solution, and adding the thiourea/ethylenediamine solution into the Cd prepared in the step (5)2+/Ti3C2Uniformly mixing the mixed solution;
(6) pouring the mixed solution prepared in the step (5) into a reactor for hydrothermal reaction, and then cooling, centrifugally washing and vacuum drying to obtain CdS/Ti3C2A catalyst.
2. The method according to claim 1, wherein the hydrofluoric acid solution in step (1) is 40% by weight, and the hydrofluoric acid solution is mixed with Ti3AlC2The volume-mass ratio is 8-12 mL/g.
3. The method according to claim 1, wherein the reactor in the step (1) and the step (5) is an uncovered polytetrafluoroethylene reaction kettle.
4. The method according to claim 1, wherein Ti is used in the step (1)3AlC2Slowly adding hydrofluoric acid solution, and reacting at constant temperature of 35-45 deg.C.
5. The method according to claim 1, wherein the drying temperature of the material in the step (3) is 45 to 55 ℃.
6. The method according to claim 1, wherein Ti is used in the step (4)3C2The mass-volume ratio of the powder to the ethylenediamine solution is 0.3-3mg/mL, and the molar volume ratio of the cadmium nitrate to the ethylenediamine solution is 0.5-1 mmol/mL.
7. The method according to claim 1, wherein Ti is used in the step (4)3C2The volume ratio of the solution of the ethylene diamine to the solution of the cadmium nitrate to the solution of the ethylene diamine is 2-4:1-3, and the mixing mode is that the solution of the cadmium nitrate to the solution of the ethylene diamine is slowly dripped into Ti3C2In the solution of ethylene diamine, adding a catalyst,mixing by ultrasonic or stirring.
8. The preparation method of claim 1, wherein the molar volume ratio of thiourea to ethylenediamine in the step (5) is 1.8-2.1mmol/mL, the solution is added by slow pouring, Cd2+/Ti3C2The volume ratio of the ethylenediamine solution to the thiourea/ethylenediamine solution is 4-6:1-3, and the mixing mode is stirring and mixing.
9. The preparation method as set forth in claim 1, wherein the hydrothermal reaction temperature in the step (6) is 150 ℃ and 170 ℃, and the reaction time is 20-26 h.
10. The one-dimensional CdS nanorod/three-dimensional multilayer Ti prepared by the preparation method of claim 13C2A composite photocatalyst is provided.
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