CN115739140A - Preparation method of bismuth vanadate/black phosphorus quantum dot composite photocatalyst - Google Patents
Preparation method of bismuth vanadate/black phosphorus quantum dot composite photocatalyst Download PDFInfo
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- 229910052720 vanadium Inorganic materials 0.000 description 1
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- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a preparation method of a bismuth vanadate/black phosphorus quantum dot composite photocatalyst, which comprises the following steps: 1) Preparing a bismuth vanadate mixed solution; 2) Adding a black phosphorus quantum dot solution into the bismuth vanadate mixed solution, uniformly mixing, and then carrying out hydrothermal reaction to obtain the bismuth vanadate/black phosphorus quantum dot composite photocatalyst. The bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared by the invention has the advantages of small band gap, low cost, good dispersibility, no toxicity, corrosion resistance and response to visible light, so that the bismuth vanadate/black phosphorus quantum dot composite photocatalyst has important application value in the fields of photocatalysis, electrocatalysis, energy storage and the like.
Description
Technical Field
The invention belongs to the field of photocatalysis. More specifically, the invention relates to a preparation method of a bismuth vanadate/black phosphorus quantum dot composite photocatalyst.
Background
In recent years, bismuth vanadate has proved to be one of promising photocatalysts, has the advantages of narrow forbidden band width (Eg =2.4 eV), no toxicity, harmlessness, visible light response and the like, can realize degradation of organic pollutants and water decomposition under the drive of visible light, and is widely concerned by researchers. Bismuth vanadate has three crystal structures: respectively a tetragonal zircon phase, a tetragonal white tungsten phase and a monoclinic white tungsten phase. Wherein, compared with other two crystal structures, the monoclinic scheelite-type bismuth vanadate has the narrowest band gap energy (2.4 eV), and has the most prominent photocatalytic activity under the irradiation of visible light. However, there is a problem that the recombination rate of photogenerated carriers is high. Therefore, further modification of bismuth vanadate is required to improve its photocatalytic activity. The photocatalytic activity of the photocatalyst can be remarkably improved by constructing the heterojunction, and the structure attributable to the heterojunction can effectively promote the transfer and separation of photon-generated carriers. Bismuth vanadate has been successfully assembled with other semiconductor photocatalysts into heterojunction structures such as: cobalt oxide/bismuth vanadate, bismuth vanadate/carbon quantum dots/cadmium sulfide, carbon quantum dots/bismuth vanadate and bismuth vanadate/graphite nitride quantum dots/nitrogen-doped carbon quantum dots.
The black phosphorus, a single-element two-dimensional layered material, is considered as a new star in the post-graphene era, and has a wide prospect in the fields of electrons, photoelectrons, biomedicine, catalysis, energy storage and the like because of having a direct band gap depending on a layer of 0.3-1.5 eV, a strong light-substance interaction and high hole mobility. When the transverse size of the black phosphorus is reduced to be below 20nm, the zero-dimensional black phosphorus quantum dot is formed, and besides the specificity of the blocky black phosphorus is inherited, the black phosphorus quantum dot has the advantages of larger surface area, more active sites, less mechanical fracture, high absorption efficiency, remarkable edge and quantum confinement effects and short carrier transport distance. Thus, the coupling of quantum dots and nanoplates (zero-dimensional and two-dimensional) may produce synergistic effects such as broadband light absorption, spatial separation of photoexcited carriers, and the like. In particular, the behaviors presented by zero-dimensional-two-dimensional mixed-dimensional hybridization are beneficial to solar fuel power generation, such as photocatalytic water splitting hydrogen production and organic pollutant degradation, and the behavior is an effective way for solving the problems of energy and environment, and is environmentally-friendly and sustainable.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and to provide at least the advantages described hereinafter.
The invention aims to provide a preparation method of a bismuth vanadate/black phosphorus quantum dot composite photocatalyst, and the prepared bismuth vanadate/black phosphorus quantum dot composite photocatalyst has the advantages of small band gap, low cost, good dispersibility, no toxicity, corrosion resistance and response to visible light, so that the bismuth vanadate/black phosphorus quantum dot composite photocatalyst has important application value in the fields of photocatalysis, electrocatalysis, energy storage and the like.
To achieve these objects and other advantages, the present invention provides a method for preparing a bismuth vanadate/black phosphorus quantum dot composite photocatalyst, comprising the following steps:
1) Preparing a bismuth vanadate mixed solution;
2) Adding a black phosphorus quantum dot solution into the bismuth vanadate mixed solution, uniformly mixing, and then carrying out hydrothermal reaction to obtain the bismuth vanadate/black phosphorus quantum dot composite photocatalyst.
Preferably, the method for preparing the bismuth vanadate mixed solution is that 0.5-5mmol of bismuth nitrate pentahydrate and 1-10g/L of sodium dodecyl benzene sulfonate are added into 20-100mL of ultrapure water to form a mixed solution I, and 0.5-5mmol of ammonium metavanadate is added into the mixed solution I to be uniformly mixed, so as to obtain the bismuth vanadate mixed solution.
Preferably, the mixed solution I is subjected to ultrasonic dispersion for 10-15min, stirring is carried out after the ultrasonic treatment is finished, the stirring rotating speed is 140-150rad/min, the stirring time is 30-50min, ammonium metavanadate is added in the stirring process to obtain a mixed solution II, nitrogen is blown into the mixed solution II, and the blowing time is 30-50min, so that a bismuth vanadate mixed solution is obtained.
Preferably, the black phosphorus quantum dot solution with the volume of 100-1000uL and the concentration of 0.5-1mg/mL is added into 20-100mL of bismuth vanadate mixed solution.
Preferably, the black phosphorus quantum dot solution is added into the bismuth vanadate mixed solution to obtain a mixed solution III, the mixed solution III is stirred at the stirring speed of 140-150rad/min for 30-50min, and ultrasonic treatment is performed for 30-50min after the stirring is finished.
Preferably, the hydrothermal reaction temperature is 175-185 ℃ and the reaction time is 5-7h.
Preferably, the yellow precipitated product obtained from the hydrothermal reaction is sequentially centrifuged, washed and dried.
Preferably, the rotation speed of the centrifugation is 10000-13000rad/min, and the centrifugation time is 10-15min.
Preferably, the washing method is to wash the resulting yellow precipitate 3 to 5 times with anhydrous ethanol and ultrapure water, respectively.
Preferably, the drying method is drying for 12-20h by using a freeze dryer.
The invention at least comprises the following beneficial effects:
firstly, the bismuth vanadate/black phosphorus quantum dot composite photocatalyst is prepared by a hydrothermal method, and the photocatalyst is excellent in photocatalytic performance and good in chemical stability. The bismuth source and the vanadium source used in the invention have rich sources, low cost and simple preparation process, and the whole preparation process of the invention has no pollution, is nontoxic, green and environment-friendly and can be prepared in large quantities.
Secondly, the bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared by the method has the advantages of small band gap, low cost, good dispersibility, no toxicity, corrosion resistance and response to visible light, and has important application value in the fields of photocatalysis, electrocatalysis, energy storage and the like.
Thirdly, the bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared by the method has excellent organic pollutant decontamination capability.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a representation diagram of the ultraviolet-visible light diffuse reflection spectrum of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst of the present invention;
FIG. 2 shows the (ahv) of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst of the invention 2 Graph of photon energy (hv);
FIG. 3 is a fluorescence spectrum of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst of the present invention;
FIG. 4 is an electrochemical impedance spectrum of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst of the present invention;
FIG. 5 is a graph showing XRD test results of different photocatalysts;
FIG. 6 is a graph of the results of degradation of rhodamine B by different photocatalysts.
Detailed Description
The present invention is described in further detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
It should be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials described therein are commercially available unless otherwise specified.
A preparation method of a bismuth vanadate/black phosphorus quantum dot composite photocatalyst comprises the following steps:
1) Preparing a bismuth vanadate mixed solution;
2) And adding a black phosphorus quantum dot solution into the bismuth vanadate mixed solution, uniformly mixing, and carrying out hydrothermal reaction to obtain the bismuth vanadate/black phosphorus quantum dot composite photocatalyst.
In another technical scheme, the method for preparing the bismuth vanadate mixed solution comprises the steps of adding 0.5-5mmol of bismuth nitrate pentahydrate and 1-10g/L of sodium dodecyl benzene sulfonate into 20-100mL of ultrapure water to form a mixed solution I, adding 0.5-5mmol of ammonium metavanadate into the mixed solution I, and uniformly mixing to obtain the bismuth vanadate mixed solution.
In another technical scheme, the mixed solution I is subjected to ultrasonic dispersion for 10-15min, stirring is carried out after the ultrasonic treatment is finished, the stirring speed is 140-150rad/min, the stirring time is 30-50min, ammonium metavanadate is added in the stirring process to obtain a mixed solution II, nitrogen is blown into the mixed solution II, and the blowing time is 30-50min, so that a bismuth vanadate mixed solution is obtained.
In another technical scheme, black phosphorus quantum dot solution with the volume of 100-1000uL and the concentration of 0.5-1mg/mL is added into 20-100mL of bismuth vanadate mixed solution.
In another technical scheme, the black phosphorus quantum dot solution is added into the bismuth vanadate mixed solution to obtain a mixed solution III, the mixed solution III is stirred at the stirring speed of 140-150rad/min for 30-50min, and ultrasonic treatment is performed for 30-50min after stirring is finished.
In another technical scheme, the temperature of the hydrothermal reaction is 175-185 ℃, and the reaction time is 5-7h.
In another technical scheme, the yellow precipitate obtained by the hydrothermal reaction is sequentially centrifuged, washed and dried.
In another technical scheme, the rotating speed of the centrifugation is 10000-13000rad/min, and the centrifugation time is 10-15min.
In another technical scheme, the washing method is to wash the obtained yellow precipitate for 3-5 times by respectively adopting absolute ethyl alcohol and ultrapure water.
In another technical scheme, the drying method is to use a freeze dryer to dry for 12-20h.
< example 1>
A preparation method of a bismuth vanadate/black phosphorus quantum dot composite photocatalyst comprises the following steps:
step one, adding 1mmol of bismuth nitrate pentahydrate and 2.0g/L of sodium dodecyl benzene sulfonate into 20mL of ultrapure water to form a mixed solution I, performing ultrasonic dispersion on the mixed solution I, wherein the ultrasonic frequency is 33KHz, the ultrasonic time is 10min, after the ultrasonic treatment is finished, performing magnetic stirring at the speed of 150rad/min, adding 1mmol of ammonium metavanadate in the stirring process to form a mixed solution II, continuously stirring the obtained mixed solution II at the rotating speed of 150rad/min for 30min, blowing nitrogen into the mixed solution II after the stirring is finished, and the blowing time is 30min;
step two, adding 200 mu L of 0.5mg/mL black phosphorus quantum dot solution into the mixed solution II after blowing nitrogen to obtain mixed solution III, carrying out magnetic stirring on the mixed solution III at the rotating speed of 150rad/min for 30min, and finally carrying out ultrasonic treatment for 30min at the ultrasonic power of 33 KHz;
step three, uniformly stirring the mixed solution III after ultrasonic dispersion, putting the mixed solution into a polytetrafluoroethylene inner container of a hydro-thermal synthesis reaction kettle, putting the hydro-thermal synthesis reaction kettle into a thermostat for reaction, and reacting for 6 hours at the reaction temperature of 180 ℃ to obtain yellow suspension;
step four, centrifuging the yellow suspension for 10min at the rotating speed of 10000rad/min to obtain yellow precipitate, respectively washing the obtained yellow precipitate for 3 times by adopting absolute ethyl alcohol and ultrapure water, and finally, placing the yellow precipitate in a freeze dryer to dry for 12h to obtain the bismuth vanadate/black phosphorus quantum dot composite photocatalyst, namely BiVO 4 /BP-200。
< example 2>
The difference from the example 1 is that 400 μ L of 0.5mg/mL black phosphorus quantum dot solution is added into the mixed solution II in the second step. The bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in this example, biVO 4 /BP-400。
< example 3>
The difference from the example 1 is that 600 μ L of 0.5mg/mL black phosphorus quantum dot solution is added into the mixed solution II in the second step. The bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in this example, biVO 4 /BP-600。
< example 4>
The difference from the example 1 is that in the second step, 800. Mu.L of 0.5mg/mL black phosphorus quantum dot solution is added into the mixed solution II. The bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in this example, biVO 4 /BP-800。
< example 5>
The difference from example 1 is that in step two 1000uL 0.5mg/ml are added to the mixture IImL black phosphorus quantum dots solution. The bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in this example, biVO 4 /BP-1000。
< example 6>
A method for photocatalytic degradation of rhodamine B by using a bismuth vanadate/black phosphorus quantum dot composite photocatalyst comprises the following steps:
step one, preparing a standard rhodamine B aqueous solution, weighing 2.5mg of rhodamine B powder, adding the rhodamine B powder into a beaker, adding proper ultrapure water to completely dissolve the rhodamine B powder, carefully transferring the rhodamine B powder into a 50mL volumetric flask by using a glass rod, finally fixing the volume and shaking up to prepare 50mL 10mg/L rhodamine B aqueous solution;
step two, 2.0g/L of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in the embodiment 4 is added into 50mL of 10mg/L rhodamine B aqueous solution to carry out a photocatalytic degradation experiment. A 300W xenon lamp (. Lamda. >420 nm) was used as a light source and placed at a distance of 10cm from the reactor, and the whole reaction process was carried out at room temperature (25 ℃); before illumination, the suspension is stirred for 20min in the dark, so that desorption-adsorption balance is achieved between the photocatalyst and RhB; turning on a light source, taking out 4mL of suspension at a fixed time interval, and centrifuging at 10000rad/min for 5min to remove photocatalyst particles to obtain a clarified rhodamine B solution;
step three, during the photodegradation, the absorbance of RhB was measured at λ =554nm by using a UV-2600 UV-vis spectrophotometer.
< comparative example 1>
The difference from example 1 is that 0. Mu.L of 0.5mg/mL black phosphorus quantum dot solution was added to the mixture II after blowing nitrogen in step two. The bismuth vanadate photocatalyst prepared in this example, biVO 4 。
< comparative example 2>
The difference from example 6 is that the bismuth vanadate photocatalyst prepared in comparative example 1 was added in the second step.
< Effect test >
< test one >
Ultraviolet and visible light diffuse reflection spectroscopy was performed on the bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in examples 1 to 5 and the bismuth vanadate photocatalyst prepared in comparative example 1, using barium sulfate as a reflectance standard, and the wavelength sweep range was 200 to 800nm, and the results are shown in fig. 1, fig. 2, and table 1.
TABLE 1
Absorption edge (nm) | Band gap (eV) | |
Example 1 | 530 | 2.43 |
Example 2 | 531 | 2.42 |
Example 3 | 532 | 2.41 |
Example 4 | 533 | 2.41 |
Example 5 | 526 | 2.44 |
Comparative example 1 | 523 | 2.45 |
As can be seen from the results of fig. 1 and fig. 2, the ultraviolet-visible diffuse reflection absorption spectra of the bismuth vanadate/black phosphorus quantum dot composite photocatalysts prepared in examples 1 to 5 with different ratios are significantly red-shifted, and the band gaps of all the photocatalysts are calculated according to the Kubelka-Munk function, and the results are shown in table 1.
< test two >
The separation and migration rates of photo-generated electron-hole pairs of the bismuth vanadate/black phosphorus quantum dot composite catalysts prepared in examples 1 to 5 and the bismuth vanadate/black phosphorus quantum dot composite catalysts prepared in comparative example 1 can be characterized by photoluminescence spectra, and the results are shown in fig. 3. The stronger the fluorescence intensity is, the lower the separation rate of the photo-generated electron-hole pairs is, and the poorer the photocatalytic performance of the photocatalyst is. BiVO prepared in comparative example 1 4 The fluorescence intensity of the photocatalyst is strongest, which indicates that the photocatalytic performance of the photocatalyst is the worst. BiVO prepared in comparative example 1 4 Compared with the photocatalyst, the fluorescence intensity of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in the embodiments 1 to 5 with different proportions is reduced, which indicates that the introduction of the black phosphorus quantum dots can effectively inhibit the recombination of electron hole pairs, thereby enhancing the photocatalytic activity of the bismuth vanadate.
< test III >
The separation and migration rates of photo-generated electron hole pairs of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in examples 1 to 5 and the bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in comparative example 1 can be further analyzed by an electrochemical impedance spectroscopy, and the results are shown in fig. 4. The nyquist semi-circle radius represents the interface charge transfer resistance, and the smaller the radius, the smaller the charge transfer resistance, the easier the charge transfer. Photocatalysts prepared in comparative example 1 and examples 1 to 5, such as BiVO, were fitted by equivalent circuit 4 ,BiVO 4 /BP-200,BiVO 4 /BP-400,BiVO 4 /BP-600,BiVO 4 /BP-800 and BiVO 4 The interface charge transfer resistances of/BP-1000 were 199.0. Omega., 118.6. Omega., 101.1. Omega., 73.9. Omega., 47.1. Omega., 78.7. Omega., respectively. BiVO prepared in comparative example 1 4 Compared with the photocatalyst, the charge transfer resistance of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in the embodiments 1 to 5 with different proportions is reduced, and the result shows that the introduction of the black phosphorus quantum dots can effectively reduce the interface resistance of the bismuth vanadate, thereby effectively promoting the separation of electron hole pairs and improving the photocatalytic performance of the bismuth vanadate.
< test four >
XRD tests were performed on the photocatalysts prepared in example 4 and comparative example 1, and the results are shown in fig. 5. The particle size of the bismuth vanadate is calculated according to the Scherrer equation, the particle size of the bismuth vanadate prepared in comparative example 1 is 28.2nm, and the particle size of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared in the invention is 25.28nm. According to the invention, the black phosphorus quantum dots are loaded on the bismuth vanadate, so that the aggregation of the bismuth vanadate is prevented, and the growth of bismuth vanadate grains is inhibited.
< test five >
The results of photodegradation of rhodamine B in example 6 and comparative example 2 are shown in fig. 6. The degradation rate of rhodamine B is calculated according to Lambert-beer law, and the formula is as follows: eta% = (1-C) t /C 0 )×100%。
The degradation rate of the rhodamine B aqueous solution in comparative example 2 was 62.6%. Example 6 has 100% of degradation rate on rhodamine B water solution. The bismuth vanadate/black phosphorus quantum dot composite photocatalyst prepared by the method can obviously improve the photocatalytic degradation of rhodamine B aqueous solution.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (10)
1. The preparation method of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst is characterized by comprising the following steps of:
1) Preparing a bismuth vanadate mixed solution;
2) And adding a black phosphorus quantum dot solution into the bismuth vanadate mixed solution, uniformly mixing, and carrying out hydrothermal reaction to obtain the bismuth vanadate/black phosphorus quantum dot composite photocatalyst.
2. The method for preparing a bismuth vanadate/black phosphorus quantum dot composite photocatalyst as claimed in claim 1, wherein the method for preparing the bismuth vanadate mixed solution is to add 0.5-5mmol of bismuth nitrate pentahydrate and 1-10g/L of sodium dodecyl benzene sulfonate into 20-100mL of ultrapure water to form a mixed solution I, add 0.5-5mmol of ammonium metavanadate into the mixed solution I, and mix uniformly to obtain the bismuth vanadate mixed solution.
3. The preparation method of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst according to claim 2, wherein the mixed solution I is subjected to ultrasonic dispersion for 10-15min, stirring is performed after the ultrasonic treatment is finished, the stirring speed is 140-150rad/min, the stirring time is 30-50min, ammonium metavanadate is added in the stirring process to obtain a mixed solution II, nitrogen is blown into the mixed solution II, and the blowing time is 30-50min, so that a bismuth vanadate mixed solution is obtained.
4. The method for preparing a bismuth vanadate/black phosphorus quantum dot composite photocatalyst according to claim 1, wherein a black phosphorus quantum dot solution with a volume of 100-1000uL and a concentration of 0.5-1mg/mL is added into 20-100mL of bismuth vanadate mixed solution.
5. The method for preparing the bismuth vanadate/black phosphorus quantum dot composite photocatalyst according to claim 1, wherein the black phosphorus quantum dot solution is added into the bismuth vanadate mixed solution to obtain a mixed solution III, the mixed solution III is stirred at a stirring speed of 140-150rad/min for 30-50min, and ultrasonic treatment is performed for 30-50min after stirring is finished.
6. The method for preparing a bismuth vanadate/black phosphorus quantum dot composite photocatalyst as claimed in claim 1, wherein the temperature of the hydrothermal reaction is 175-185 ℃, and the reaction time is 5-7h.
7. The method for preparing the bismuth vanadate/black phosphorus quantum dot composite photocatalyst according to claim 1, wherein a yellow precipitate obtained by the hydrothermal reaction is sequentially centrifuged, washed and dried.
8. The method for preparing a bismuth vanadate/black phosphorus quantum dot composite photocatalyst as claimed in claim 7, wherein the centrifugation rotation speed is 10000-13000rad/min, and the centrifugation time is 10-15min.
9. The method for preparing the bismuth vanadate/black phosphorus quantum dot composite photocatalyst as claimed in claim 7, wherein the washing method comprises washing the obtained yellow precipitate 3-5 times with anhydrous ethanol and ultrapure water respectively.
10. The preparation method of the bismuth vanadate/black phosphorus quantum dot composite photocatalyst as claimed in claim 7, wherein the drying method is drying for 12-20 hours by using a freeze dryer.
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