A conical TiO2 / CdSe photocatalyst and a preparation method thereof

Abstract

The application discloses a conical TiO2 / CdSe photocatalyst and a preparation method thereof. The method comprises the following steps: firstly, using isopropyl titanate as a titanium source, nano conical TiO2 is prepared on a titanium mesh substrate by a hydrothermal method; using CdCl2 and SeO2 as raw materials, nano spherical CdSe is prepared by a three-electrode system electrochemical deposition method; using the titanium mesh on which the TiO2 nano cone grows as a working electrode, and using CdCl2 and SeO2 as raw materials, conical TiO2 / CdSe composite materials are prepared by electrochemical deposition. The heterostructure constructed in the composite materials promotes the separation and migration of photo-generated carriers, and can effectively remove antibiotic pollutants in water and decompose water to generate H2 fuel.

Description

Technical Field

[0001] This invention relates to the field of materials technology, specifically to a cone-shaped TiO2 / CdSe photocatalyst and its preparation method. Background Technology

[0002] The water pollution problem caused by antibiotic overuse is particularly prominent. The wastewater is characterized by high biotoxicity and the presence of antibacterial substances. Traditional physical adsorption and biological treatment methods are ineffective in treating this type of recalcitrant toxic organic wastewater. With fossil fuel resources dwindling and their use causing environmental pollution, the development of efficient and clean energy technologies such as H2 is urgently needed. Photocatalysis is an environmental remediation technology with broad development prospects. Utilizing semiconductor photocatalysts, under ultraviolet-visible light irradiation, the semiconductor is excited to generate electron-hole pairs. Taking advantage of its redox properties, active groups are generated to degrade antibiotics into small molecule products such as H2O and CO2, and to decompose water to produce H2. It has the advantages of mild reaction, simple operation, and reusability, and has good scientific research value and economic benefits.

[0003] TiO2 is an excellent semiconductor material with advantages such as high redox potential, high reactivity, high efficiency, chemical stability, non-toxicity, ease of synthesis, and low cost, playing a vital role in photocatalysis. However, conventionally morphological TiO2 exhibits low photogenerated electron-hole pair separation efficiency and few reactive sites, resulting in insufficient photocatalytic activity. Furthermore, its wide photocatalytic bandgap of approximately 3.2 eV limits its light absorption, allowing it to absorb only 5% of the ultraviolet energy of the solar spectrum, significantly restricting the photocatalytic efficiency of TiO2. Summary of the Invention

[0004] The purpose of this invention is to provide a cone-shaped TiO2 / CdSe photocatalyst and its preparation method, which can improve photocatalytic efficiency.

[0005] In one aspect of the invention, a method for preparing a cone-shaped TiO2 / CdSe photocatalyst is provided. According to an embodiment of the invention, CdSe is deposited in an electrolyte using cyclic voltammetry in a three-electrode system, followed by washing, drying, and annealing to obtain the cone-shaped TiO2 / CdSe composite material. In the three-electrode system, a titanium mesh with nano-conical TiO2 grown on it is used as the working electrode.

[0006] In addition, the ternary cathode material precursor according to the above embodiments of the present invention may also have the following additional technical features:

[0007] In some embodiments of the present invention, the method for preparing the titanium mesh with nano-conical TiO2 includes the following steps: adding a mixed solution of acetylacetone and isopropyl titanate to a disodium ethylenediaminetetraacetate solution, stirring until the solution is transparent, using the Ti mesh as a substrate, carrying out a hydrothermal reaction, and then washing, drying, and annealing to obtain nano-conical TiO2.

[0008] In some embodiments of the present invention, the solubility of the disodium ethylenediaminetetraacetate solution is 0.075 to 0.080 mol / L, and the volume ratio of the disodium ethylenediaminetetraacetate, acetylacetone, and isopropyl titanate is 18 to 20:2:0.3.

[0009] In some embodiments of the present invention, during the preparation of nanoconical TiO2: the Ti mesh is ultrasonically cleaned for 20-30 minutes each with acetone, isopropanol, ethanol, and deionized water before the hydrothermal reaction; the hydrothermal reaction temperature is 200-220°C, and the hydrothermal reaction holding time is 5-5.5 h; the washing after the hydrothermal reaction is done with water and ethanol; the drying temperature is 50-60°C, and the drying time is 10-20 min; the initial annealing temperature is 30-50°C, the heating rate is 2-5°C / min, and the annealing temperature is maintained at 500-600°C for 1-2 h.

[0010] In some embodiments of the present invention, the preparation method of CdSe includes the following steps: adjusting the pH of the electrolyte to 3, depositing CdSe on a titanium mesh in a three-electrode system using cyclic voltammetry, washing, drying, and annealing the sample to obtain nanospheres of CdSe, wherein the electrolyte includes cadmium chloride, selenium dioxide, and sodium tartrate.

[0011] In some embodiments of the present invention, the concentrations of cadmium chloride, selenium dioxide, and sodium tartrate are 0.1–0.15 mol / L, 0.4–0.6 mmol / L, and 0.01–0.015 mol / L, respectively.

[0012] In some embodiments of the present invention, during the preparation of CdSe: the three-electrode system uses a Ti mesh as the working electrode, a saturated calomel electrode as the reference electrode, and a Pt electrode as the counter electrode; the cyclic voltammetry deposition potential is -0.3V to -0.9V Vs.SCE, the scan rate is 10 to 15mV / s, and the total deposition time is 120 to 480s; the washing is performed using water; the drying temperature is 50 to 60℃, and the time is 10 to 20min; the annealing process is carried out in a tube furnace under N2 atmosphere, with an initial temperature of 30 to 50℃, a heating rate of 2 to 5℃ / min, and a holding time of 200 to 250℃ for 2 to 3 hours.

[0013] In some embodiments of the present invention, in the three-electrode system, a saturated calomel electrode is used as the reference electrode and a Pt electrode is used as the counter electrode; the cyclic voltammetry deposition potential is -0.3V to -0.9V Vs.SCE, the scan rate is 10 to 15mV / s, and the total deposition time is 120 to 480s; the electrolyte includes cadmium chloride, selenium dioxide, and sodium tartrate, and the concentrations of cadmium chloride, selenium dioxide, and sodium tartrate are 0.1 to 0.15 mol / L, 0.4 to 0.6 mmol / L, and 0.01 to 0.015 mol / L, respectively.

[0014] In some embodiments of the present invention, the washing is performed using water; the drying temperature is 50-60°C and the time is 10-20 min; the annealing process is carried out in a tube furnace under N2 atmosphere, with an initial temperature of 30-50°C, a heating rate of 2-5°C / min, and a holding time of 200-250°C for 2-3 h.

[0015] In another aspect of the present invention, a conical TiO2 / CdSe photocatalyst prepared according to the aforementioned method for preparing the conical TiO2 / CdSe photocatalyst is provided.

[0016] In another aspect of the invention, the present invention proposes the application of the aforementioned cone-shaped TiO2 / CdSe photocatalyst. According to embodiments of the invention, the cone-shaped TiO2 / CdSe photocatalyst is used to degrade antibiotics and decompose water to produce H2.

[0017] Compared with the prior art, the beneficial effects of the present invention are:

[0018] This invention prepares a cone-shaped TiO2 / CdSe photocatalyst using a simple hydrothermal and electrochemical deposition method. The nanocone array structure can effectively promote the separation of photogenerated electron-hole pairs and provide more active sites for photocatalytic reactions, thereby effectively improving the photocatalytic performance of the material.

[0019] The composite material of CdSe broadens the light absorption range of the catalyst into the visible light range. Combined with TiO2, it forms a heterostructure, thus avoiding the recombination of photogenerated electron-hole pairs. This allows for effective separation and migration of photogenerated charges, enhancing the photocatalytic activity of the material. Under light excitation, electrons in the valence bands of TiO2 and CdSe are excited to transition to the conduction band, leaving holes in the valence band, thereby generating photogenerated electron-hole pairs. Since the conduction band potential of TiO2 is more positive than that of CdSe, and its valence band potential is also more positive, the band structures in the composite material TiO2 / CdSe are matched, forming a heterostructure. Therefore, photogenerated electrons accumulate in the conduction band of TiO2, while photogenerated holes accumulate in the valence band of CdSe. The conduction band position of TiO2 is higher than that of O2 / ·O2. -Its potential is more negative, and the excited electrons can react with O2 to produce a highly oxidizing reactive substance, O2. - In photocatalysis, TiO2 can effectively degrade antibiotics such as tetracycline hydrochloride. Meanwhile, the conduction band position of TiO2 is higher than that of H... + The potential of O2 / H2O is more negative, and the valence band position of CdSe is more positive than that of O2 / H2O, which can efficiently decompose water to produce H2 fuel during photocatalysis. Attached Figure Description

[0020] Figure 1 This is a flowchart illustrating the preparation process of the cone-shaped TiO2 / CdSe photocatalyst in Example 1 of the present invention;

[0021] Figure 2 The XRD patterns of TiO2, CdSe, and conical TiO2 / CdSe photocatalysts in Example 1 of this invention are shown below.

[0022] Figure 3 The images shown are SEM images of the photocatalyst in Example 1 of this invention. (a) and (b) are cone-shaped TiO2 at different magnifications, (c) and (d) are spherical CdSe at different magnifications, and (e) and (f) are TiO2 / CdSe at different magnifications.

[0023] Figure 4 The UV-Vis DRS spectra of TiO2, CdSe, and conical TiO2 / CdSe photocatalysts in Example 1 of this invention are shown.

[0024] Figure 5 The image shows the it spectrum of TiO2 and conical TiO2 / CdSe photocatalyst in Example 1 of this invention;

[0025] Figure 6 The EIS spectra of TiO2 and conical TiO2 / CdSe photocatalyst in Example 1 of this invention are shown.

[0026] Figure 7 The LSV spectra of TiO2 and conical TiO2 / CdSe photocatalyst in Example 1 of this invention are shown.

[0027] Figure 8 The graphs show the degradation of tetracycline hydrochloride by TiO2 and conical TiO2 / CdSe photocatalyst in Example 1 of this invention, including (a) degradation concentration variation graph and (b) degradation kinetic graph.

[0028] Figure 9 The figures show the hydrogen production from water splitting using TiO2 and the conical TiO2 / CdSe photocatalyst in Example 1 of this invention: (a) hydrogen production from water splitting and (b) hydrogen production rate from water splitting. Detailed Implementation

[0029] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0030] Example 1

[0031] A method for preparing a cone-shaped TiO2 / CdSe photocatalyst includes the following steps:

[0032] (1) Preparation of conical TiO2

[0033] Use a 100-mesh titanium mesh with dimensions of 20mm*30mm*0.27mm. Clean it with acetone, isopropanol, ethanol, and deionized water for 30 minutes each. Place the cleaned titanium mesh diagonally into a 50ml polytetrafluoroethylene inner liner.

[0034] A 0.075 mol / L solution of disodium ethylenediaminetetraacetate (Na2EDTA) was prepared. 18 mL of this solution was placed in a beaker, and a mixture of 2 mL of acetylacetone (ACAC) and 0.3 mL of isopropyl titanate was added dropwise at a uniform rate. The mixture was stirred continuously at room temperature for 1 hour until the solution turned yellow and transparent. The solution was then transferred to a polytetrafluoroethylene (PTFE) liner and subjected to hydrothermal reaction at 200 °C for 5 hours using a Ti mesh as a substrate. The sample was washed repeatedly with water and ethanol, and dried at 60 °C for 10 minutes. The sample was then transferred to a crucible and annealed in a box furnace at 500 °C for 2 hours (initial temperature 30 °C, heating rate 2 °C / min). The sample was collected, yielding a titanium mesh with nano-conical TiO2 grown on it.

[0035] (2) Preparation of spherical CdSe

[0036] An electrolyte containing 0.1 mol / L cadmium chloride (CdCl2), 0.4 mmol / L selenium dioxide (SeO2), and 0.01 mol / L sodium tartrate (C4H4Na2O6) was prepared, and the pH was adjusted to 3 with concentrated hydrochloric acid. A three-electrode system was used for electrochemical deposition: a cleaned Ti mesh as the working electrode, a saturated calomel electrode as the reference electrode, and a Pt electrode as the counter electrode. Cyclic voltammetry was used, with an initial deposition potential of -0.3 V, a final deposition potential of -0.9 V (Vs.SCE), a scan rate of 10 mV / s, and a total deposition time of 240 s. The sample was washed repeatedly with water, dried at 60 °C for 10 min, then transferred to a crucible and annealed in a tube furnace under N2 atmosphere at 200 °C for 2 h (initial temperature 30 °C, heating rate 2 °C / min). The sample was collected to obtain nanospheres of CdSe.

[0037] (3) Preparation of TiO2 / CdSe

[0038] An electrolyte containing 0.1 mol / L cadmium chloride (CdCl2), 0.4 mmol / L selenium dioxide (SeO2), and 0.01 mol / L sodium tartrate (C4H4Na2O6) was prepared, and the pH was adjusted to 3 with concentrated hydrochloric acid. A three-electrode system was used for electrochemical deposition: a Ti mesh with nanoconical TiO2 as the working electrode, a saturated calomel electrode as the reference electrode, and a Pt electrode as the counter electrode. Cyclic voltammetry was used, with an initial deposition potential of -0.3 V, a final deposition potential of -0.9 V (Vs.SCE), a scan rate of 10 mV / s, and a total deposition time of 240 s. The sample was washed repeatedly with water, dried at 60 °C for 10 min, then transferred to a crucible and annealed in a tube furnace under N2 atmosphere at 200 °C for 2 h (initial temperature 30 °C, heating rate 2 °C / min). The sample was then collected, yielding the conical TiO2 / CdSe photocatalyst.

[0039] The performance of the prepared cone-shaped TiO2 / CdSe photocatalyst was analyzed.

[0040] (1) XRD analysis

[0041] The phase structures of nanoconical TiO2, nanospherical CdSe, and conical TiO2 / CdSe photocatalysts were analyzed by XRD, such as... Figure 2 As shown, the prepared nanoconical TiO2 corresponds well with the standard card PDF#21-1276. The diffraction peaks at 27.4°, 36.1°, 54.3°, and 69.8° correspond to the (110), (101), (211), and (112) crystal planes of rutile TiO2, respectively, proving that TiO2 was successfully prepared on the Ti mesh and that it is a rutile phase structure. The XRD pattern of the nanospherical CdSe is compared with the standard CdSe card PDF#08-0459. The diffraction peaks at 27.08° and 35.11° correspond to the (101) and (102) crystal planes of CdSe, respectively. In addition, the XRD pattern of the TiO2 / CdSe composite material shows the combined characteristics of TiO2 and CdSe.

[0042] (2) SEM analysis

[0043] Figure 3 (a) and (b) are SEM images of nanoconical TiO2, showing that a TiO2 nanocone array was successfully synthesized, uniformly and densely arranged vertically on a titanium mesh substrate, with a diameter of approximately 50 nm. Figure 3 (c) and (d) show that the synthesized CdSe nanospheres are uniformly distributed and have a diameter of about 50 nm. Figure 3(e) and (f) are SEM images of TiO2 / CdSe. It can be seen that CdSe nanospheres are uniformly grown on TiO2 nanocone arrays with good size matching and a certain degree of separation between particles, indicating that CdSe and TiO2 are successfully combined.

[0044] (3) UV-Vis DRS analysis

[0045] Light absorption capacity is an important indicator for evaluating the photoactivity of photocatalysts, and its light absorption range can be studied using UV-Vis DRS spectroscopy. Figure 4 As shown, the absorption spectrum of the TiO2 / CdSe photocatalyst exhibits a significant red shift compared to pure TiO2. Therefore, combining TiO2 nanocone arrays with CdSe can significantly increase its response range to visible light.

[0046] (4) IT analysis

[0047] The photocurrent-it curve can reflect the degree of response and stability of a catalyst under light irradiation. For example... Figure 5 As shown, under 10 cycles of simulated sunlight irradiation, the photocurrent density of TiO2 remained stable at 1.00 mA / cm². 2 The photocurrent density of the TiO2 / CdSe composite material is 2.34 mA / cm². 2 The value is 2.34 times that of pure TiO2, indicating that the photoelectric performance of TiO2 / CdSe is improved after composite treatment.

[0048] (5) EIS analysis

[0049] EIS test results as follows Figure 6 As shown in the EIS spectrum, the radius of curvature of the TiO2 / CdSe composite material is clearly smaller than that of TiO2. This indicates that the structure of the composite material can successfully reduce charge transfer resistance, promote effective charge separation and transport, and improve the photocatalytic activity of the material.

[0050] (6) LSV analysis

[0051] like Figure 7 As shown, comparing the LSV curves of pure TiO2 and TiO2 / CdSe, it can be seen that at a current density of 10 mA / cm²... 2 At that time, the hydrogen evolution overpotentials of the two catalysts were -1.56V and -1.42V, respectively. The higher overpotential of TiO2 (-1.56V) indicates that this electrode has a higher electron-hole recombination rate and a lower photoinduced electron transfer efficiency. The lower overpotential of TiO2 / CdSe (-1.42V) indicates that the separation efficiency of photogenerated carriers was optimized after the two catalysts were combined.

[0052] (7) Analysis of the degradation of tetracycline hydrochloride

[0053] like Figure 8 As shown in (a), almost no catalytic degradation reaction occurs within 30 min of adsorption in the dark. Under simulated sunlight, the material can effectively degrade tetracycline hydrochloride, exhibiting photocatalytic activity. The degradation rates of 5 mg / L tetracycline hydrochloride by TiO2 and TiO2 / CdSe within 2 h are 83.2% and 93.3%, respectively. Figure 8 As shown in (b), the reaction rate constants K for TiO2 and TiO2 / CdSe are 0.01623 min. -1 and 0.02219min -1 Compared with TiO2 alone, the TiO2 / CdSe composite material exhibits improved performance in photocatalytic degradation of antibiotics.

[0054] (8) Hydrogen production analysis from water decomposition

[0055] like Figure 9 As shown in (a), under simulated sunlight irradiation and an applied potential of 0.5V, the hydrogen production of TiO2 and TiO2 / CdSe within 3 h was 83.05 μmol·cm⁻¹. -2 and 166.34 μmol·cm -2 TiO2 alone exhibits poor photocatalytic activity, such as... Figure 9 As shown in (b), the activity of TiO2 / CdSe is significantly improved, and the average hydrogen production rate can reach 55.45 μmol·h within 3 h. -1 ·cm -2 It is twice that of a single TAs. The formation of heterojunctions in the composite material accelerates the separation and migration efficiency of photogenerated electron-hole pairs in the hydrogen production path, significantly improving its photoelectric conversion efficiency.

[0056] Example 2

[0057] A method for preparing a cone-shaped TiO2 / CdSe photocatalyst includes the following steps:

[0058] (1) Preparation of conical TiO2

[0059] Use a 100-mesh titanium mesh with dimensions of 20mm*30mm*0.27mm. Clean it with acetone, isopropanol, ethanol, and deionized water for 30 minutes each. Place the cleaned titanium mesh diagonally into a 50ml polytetrafluoroethylene inner liner.

[0060] A 0.075 mol / L solution of disodium ethylenediaminetetraacetate (Na2EDTA) was prepared. 18 mL of this solution was placed in a beaker, and a mixture of 2 mL of acetylacetone (ACAC) and 0.3 mL of isopropyl titanate was added dropwise at a uniform rate. The mixture was stirred continuously at room temperature for 1 hour until the solution turned yellow and transparent. The solution was then transferred to a polytetrafluoroethylene (PTFE) liner and subjected to hydrothermal reaction at 200 °C for 5 hours using a Ti mesh as a substrate. The sample was washed repeatedly with water and ethanol, and dried at 60 °C for 10 minutes. The sample was then transferred to a crucible and annealed in a box furnace at 500 °C for 1 hour (initial temperature 50 °C, heating rate 5 °C / min). The sample was collected, yielding a titanium mesh with nano-conical TiO2 grown on it.

[0061] (2) Preparation of spherical CdSe

[0062] An electrolyte containing 0.1 mol / L cadmium chloride (CdCl2), 0.4 mmol / L selenium dioxide (SeO2), and 0.01 mol / L sodium tartrate (C4H4Na2O6) was prepared, and the pH was adjusted to 3 with concentrated hydrochloric acid. A three-electrode system was used for electrochemical deposition: a cleaned Ti mesh as the working electrode, a saturated calomel electrode as the reference electrode, and a Pt electrode as the counter electrode. Cyclic voltammetry was used, with an initial deposition potential of -0.3 V, a final deposition potential of -0.9 V (Vs.SCE), a scan rate of 10 mV / s, and a total deposition time of 360 s. The sample was washed repeatedly with water, dried at 60 °C for 10 min, then transferred to a crucible and annealed in a tube furnace under N2 atmosphere at 200 °C for 2 h (initial temperature 50 °C, heating rate 5 °C / min). The sample was collected to obtain nanospheres of CdSe.

[0063] (3) Preparation of TiO2 / CdSe

[0064] An electrolyte containing 0.1 mol / L cadmium chloride (CdCl2), 0.4 mmol / L selenium dioxide (SeO2), and 0.01 mol / L sodium tartrate (C4H4Na2O6) was prepared, and the pH was adjusted to 3 with concentrated hydrochloric acid. A three-electrode system was used for electrochemical deposition: a Ti mesh with nanoconical TiO2 as the working electrode, a saturated calomel electrode as the reference electrode, and a Pt electrode as the counter electrode. Cyclic voltammetry was used, with an initial deposition potential of -0.3 V, a termination deposition potential of -0.9 V (Vs.SCE), a scan rate of 10 mV / s, and a total deposition time of 360 s. The sample was washed repeatedly with water, dried at 60 °C for 10 min, then transferred to a crucible and annealed in a tube furnace under N2 atmosphere at 200 °C for 2 h (initial temperature 50 °C, heating rate 5 °C / min). The sample was then collected, yielding the conical TiO2 / CdSe photocatalyst.

[0065] The above description is merely an example and illustration of the structure of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described or use similar methods to replace them, as long as they do not deviate from the structure of the present invention or exceed the scope defined in the claims, they should all fall within the protection scope of the present invention.

Claims

1. A method for preparing a cone-shaped TiO2 / CdSe photocatalyst, characterized in that: CdSe was deposited in an electrolyte using cyclic voltammetry in a three-electrode system, followed by washing, drying, and annealing to obtain the conical TiO2 / CdSe composite material. CdSe nanospheres were uniformly grown on a TiO2 nanocone array. In the three-electrode system, a titanium mesh with grown nanoconical TiO2 was used as the working electrode. The drying temperature was 50–60 °C for 10–20 min. The annealing process was carried out in a tube furnace under N2 atmosphere, with an initial temperature of 30–50 °C, a heating rate of 2–5 °C / min, and a holding time of 200–250 °C for 2–3 h. In the three-electrode system, the saturated calomel electrode serves as the reference electrode, and the Pt electrode serves as the counter electrode. The cyclic voltammetry deposition potential is -0.3V to -0.9V Vs.SCE, the scan rate is 10~15mV / s, and the total deposition time is 120~480s; The electrolyte comprises cadmium chloride, selenium dioxide, and sodium tartrate, wherein the concentrations of cadmium chloride, selenium dioxide, and sodium tartrate are 0.1~0.15 mol / L, 0.4~0.6 mmol / L, and 0.01~0.015 mol / L, respectively.

2. The method for preparing a cone-shaped TiO2 / CdSe photocatalyst according to claim 1, characterized in that, The method for preparing the titanium mesh with nano-conical TiO2 includes the following steps: adding a mixed solution of acetylacetone and isopropyl titanate to a disodium ethylenediaminetetraacetate solution, stirring until the solution is transparent, using the Ti mesh as a substrate, carrying out a hydrothermal reaction, and then washing, drying, and annealing to obtain nano-conical TiO2.

3. The method for preparing a cone-shaped TiO2 / CdSe photocatalyst according to claim 2, characterized in that: The solubility of the disodium ethylenediaminetetraacetate solution is 0.075~0.080 mol / L, and the volume ratio of the disodium ethylenediaminetetraacetate, acetylacetone and isopropyl titanate is 18~20:2:0.

3.

4. The method for preparing a cone-shaped TiO2 / CdSe photocatalyst according to claim 2, characterized in that, In the preparation process of nanoconical TiO2: Before the hydrothermal reaction, the Ti mesh was ultrasonically cleaned for 20-30 minutes with acetone, isopropanol, ethanol, and deionized water, respectively. The hydrothermal reaction temperature is 200~220℃, and the hydrothermal reaction holding time is 5~5.5h; The washing process following the hydrothermal reaction uses water and ethanol. The drying temperature is 50~60℃, and the time is 10~20min; The initial annealing temperature is 30~50℃, the heating rate is 2~5℃ / min, and the temperature is held at 500~600℃ for 1~2 hours.

5. The method for preparing a cone-shaped TiO2 / CdSe photocatalyst according to claim 1, characterized in that: Adjust the pH of the electrolyte to 3.

6. The method for preparing a cone-shaped TiO2 / CdSe photocatalyst according to claim 1, characterized in that: The washing process uses water.

7. A cone-shaped TiO2 / CdSe photocatalyst prepared by the method of any one of claims 1-6.

8. The application of the cone-shaped TiO2 / CdSe photocatalyst according to claim 7, characterized in that: The cone-shaped TiO2 / CdSe photocatalyst is used to degrade antibiotics and decompose water to produce H2.

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