CN113499790B - Preparation and application of uranium reduction-separated Ag-doped CdSe nanosheet photocatalytic material - Google Patents
Preparation and application of uranium reduction-separated Ag-doped CdSe nanosheet photocatalytic material Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 title claims abstract 14
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 16
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 16
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Abstract
The invention discloses a preparation and application of a uranium reduction separated Ag doped CdSe nano sheet photocatalytic material, which comprises the following steps: cdCl is reacted with 2 ·2.5H 2 O and AgNO 3 Mixing the mixed powder of (1) with a first mixed solvent of octylamine and oleylamine, heating for reaction, and cooling to room temperature to obtain a reaction solution; mixing Se powder with a second mixed solvent of octylamine and oleylamine at room temperature to obtain Se precursor solution; and adding Se precursor solution into the reaction solution, heating for reaction, cooling, washing the obtained precipitate with chloroform solution for multiple times, uniformly mixing the precipitate with cetyltrimethylammonium bromide solution, performing ultrasonic treatment, washing with ethanol, and drying to obtain the Ag doped CdSe nano-sheet photocatalytic material separated by uranium reduction. The Ag doped CdSe nano sheet photocatalytic material provided by the invention can improve the light absorption capacity and simultaneously meet the requirement of photocatalytic reduction of U (VI), and is more beneficial to generation and use of photogenerated carriers.
Description
Technical Field
The invention belongs to the technical field of inorganic nano materials and preparation thereof, and particularly relates to preparation and application of a uranium reduction-separated Ag-doped CdSe nano-sheet photocatalytic material.
Background
Nuclear energy is a relatively clean energy source that has evolved rapidly over the last decades, as compared to traditional fossil fuels, which cause serious environmental pollution and climate change. However, the reserves of uranium ores that have been ascertained on land are limited. Due to the widespread use of nuclear power, large-scale uranium mining, nuclear accident and improper disposal of nuclear waste, a large amount of radioactive uranium permeates into the environment mainly in the form of hexavalent uranium (U (VI)). Therefore, U (VI) needs to be extracted at the same time of environmental monitoring and protection. However, there are a number of technical challenges in extracting uranium from uranium-containing waste solutions due to the low concentration of uranium and the interference of a large number of coexisting ions. At present, the photocatalysis uranium reduction method is an emerging environment-friendly method, but the photocatalysis performance of a semiconductor can be influenced by factors such as light absorption wavelength, material self stability and the like. Finding a suitable energy band structure and high extraction amount of photocatalyst remains a challenge for the extraction of U (VI) in uranium-containing wastewater.
The invention takes a CdSe nano sheet with a narrow band gap as a research object, the original CdSe nano sheet is a combination of two crystal structures of sphalerite and wurtzite, and the crystal structure of the CdSe nano sheet is adjusted by doping a small amount of Ag, so that the CdSe nano sheet is mainly of sphalerite crystal structure. The change of the crystal structure reduces the band gap width of the CdSe nano sheet, and simultaneously satisfies the photocatalysis reduction of U (VI), so that the light absorption wavelength range of the 3 percent Ag-CdSe nano sheet is enlarged, and the generation and the utilization of photo-generated carriers are facilitated.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a method for preparing a uranium reduction-separated Ag doped CdSe nanoplatelet photocatalytic material, comprising the steps of:
step one, cdCl 2 ·2.5H 2 O and AgNO 3 Uniformly mixing the mixed powder of (1) with a first mixed solvent of octylamine and oleylamine, heating to 115-125 ℃, reacting for 1-3 hours, and naturally cooling to room temperature to obtain a reaction solution;
step two, uniformly mixing Se powder with a second mixed solvent of octylamine and oleylamine at room temperature to obtain Se precursor solution;
and step three, adding the Se precursor solution in the step two into the reaction solution in the step one, heating to 90-100 ℃, reacting for 14-18 hours, cooling to room temperature, washing the obtained precipitate with a chloroform solution for multiple times, uniformly mixing the precipitate with a cetyltrimethylammonium bromide solution, performing ultrasonic treatment for 45-90 min, washing the precipitate with ethanol for multiple times, and performing vacuum drying to obtain the Ag doped CdSe nano-sheet photocatalytic material.
Preferably, in the first step, cdCl 2 ·2.5H 2 O and AgNO 3 The molar ratio of (2) is 1.4-1.5:0.01-0.035; the volume ratio of the octylamine to the oleylamine is 1:1; the molar volume ratio of the mixed powder to the first mixed solvent is 1.5 mmol/10 mL.
Preferably, in the second step, the molar volume ratio of the Se powder to the second mixed solvent is 4.5mmol:5mL; the volume ratio of the octylamine to the oleylamine is 1:1; the molar ratio of the Se powder to the mixed powder in the second step is 2.5-3.5:1.
Preferably, in the third step, the concentration of the cetyltrimethylammonium bromide solution is 0.05-0.15 mol/L; the mol volume ratio of the mixed powder in the first step to the cetyltrimethylammonium bromide solution is 1.5 mmol:25-45 mL.
Preferably, in the third step, the process of ultrasonic treatment for 45-90 min after the precipitate and the cetyltrimethylammonium bromide solution are uniformly mixed is replaced by: adding the precipitate and hexadecyl trimethyl ammonium bromide solution into a supercritical carbon dioxide reaction device, injecting carbon dioxide into the supercritical carbon dioxide reaction device, stirring for 15-30 min at the temperature of 35-40 ℃ and the pressure of 12-18 MPa, decompressing, and then performing ultrasonic treatment for 15-30 min; and then washing the precipitate with ethanol for multiple times, and vacuum drying to obtain the Ag doped CdSe nano sheet photocatalytic material.
Preferably, in the third step, the obtained Ag doped CdSe nano sheet photocatalytic material is treated for 1-3 min by using a low-temperature plasma treatment instrument.
Preferably, the atmosphere of the low-temperature plasma treatment instrument is argon; the frequency of the low-temperature plasma treatment instrument is 35-45 KHz, the power is 45-60W, and the pressure of the atmosphere is 30-45 Pa.
The invention also provides an application of the uranium reduction-separated Ag-doped CdSe nano sheet photocatalytic material in radioactive wastewater treatment, which is characterized in that the radioactive wastewater is uranium-containing radioactive wastewater.
Preferably, ag doped CdSe nanosheet photocatalytic materials are added into uranium-containing radioactive wastewater, and photocatalytic reaction is carried out under the condition that a xenon lamp simulates sunlight, so that photocatalytic reduction of hexavalent uranium in the uranium-containing radioactive wastewater is realized; simultaneously, the photocatalyst material after the photocatalytic reaction is oxidized in the air for 48 hours, and then the photocatalyst material is dispersed to 0.1mol/L KHCO 3 Elution reaction is carried out in solution to remove UO deposited on the catalyst 2 And then washing with water, and drying the collected photocatalyst material for recycling.
The invention at least comprises the following beneficial effects: the invention prepares the Ag doped CdSe nano sheet, the original CdSe nano sheet is a combination of two crystal structures of sphalerite and wurtzite, and along with the doping of Ag, the wurtzite crystal structure in the CdSe nano sheet is reduced. According to the analysis of the energy band structure, the change of the crystal structure is found to reduce the band gap width of the CdSe nano sheet, improve the conduction band position of the CdSe nano sheet, ensure that the Ag-CdSe nano sheet can improve the light absorption capacity and simultaneously meet the requirement of photocatalytic reduction of U (VI), and is more beneficial to the generation and use of photogenerated carriers.
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.
Description of the drawings:
FIG. 1 is a TEM image of a uranium reduction-separated Ag-doped CdSe nanosheet photocatalytic material prepared in comparative example 1 (a) and example 2 (b) of the present invention;
FIG. 2 shows the HRTEM of the uranium reduction-separated Ag-doped CdSe nanosheet photocatalytic material prepared in comparative example 1 (a) and example 2 (b) of the present invention;
FIG. 3 is an XRD pattern of the photocatalytic materials prepared in examples 1 to 2 and comparative example 1 according to the present invention;
FIG. 4 is a Raman spectrum of the photocatalytic materials prepared in examples 1 to 2 and comparative example 1 according to the present invention;
FIG. 5 is an infrared spectrum of the photocatalytic material prepared in examples 1 to 2 and comparative example 1 according to the present invention;
FIG. 6 is an XPS spectrum of the photocatalytic materials prepared in examples 1 to 2 and comparative example 1 according to the present invention;
FIG. 7 is a graph of Mo Texiao Takara Shuzo (a) and a graph of band gap value (b) of the photocatalytic materials prepared in examples 1 to 2 and comparative example 1 according to the present invention;
FIG. 8 shows the valence band curves (a) and secondary electron edge curves (b) of UPS spectra of the photocatalytic materials prepared in examples 1 to 2 and comparative example 1 according to the present invention;
FIG. 9 is a diagram showing the energy band structure of the photocatalytic materials prepared in examples 1 to 2 and comparative example 1 according to the present invention;
FIG. 10 is a graph showing the U (VI) removal ratios of the photocatalytic materials prepared in examples 1 to 2 and comparative example 1 according to the present invention under dark conditions;
FIG. 11 is a graph showing the U (VI) removal ratios under light conditions of the photocatalytic materials prepared in examples 1 to 2 and comparative example 1 according to the present invention;
FIG. 12 is a graph showing the U (VI) removal ratios of the photocatalytic materials prepared in examples 2 to 4 according to the present invention under dark conditions;
FIG. 13 is a graph showing the U (VI) removal ratios under illumination of the photocatalytic materials prepared in examples 2 to 4 of the present invention;
FIG. 14 shows the U (VI) removal rates of the photocatalytic material prepared in example 2 under different solid-to-liquid ratios;
FIG. 15 shows the U (VI) removal rate of the photocatalytic material prepared in example 2 of the present invention in the presence of competing ions;
FIG. 16 shows the U (VI) removal ratios of the photocatalytic material prepared in example 2 of the present invention under different pH conditions;
FIG. 17 shows XPS spectra of U4 f (a), cd3d (b), se 3d (c) and Ag 3d (d) of the photocatalytic material prepared in example 2 of the present invention before and after the photocatalytic reaction;
fig. 18 shows a valence band curve (a) and a secondary electron edge curve (b) of UPS spectra of the photocatalytic material prepared in example 2 of the present invention before and after the photocatalytic reaction.
The specific embodiment is as follows:
the present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.
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.
Example 1:
the preparation method of the uranium reduction separated Ag doped CdSe nano sheet photocatalytic material comprises the following steps:
step one, 1.485mmol CdCl 2 ·2.5H 2 O and 0.015mmol AgNO 3 Uniformly mixing the mixed powder of (1) with 5mL of octylamine and 5mL of a first mixed solvent of oleylamine, heating to 120 ℃ for reaction for 2 hours, and naturally cooling to room temperature to obtain a reaction solution;
step two, uniformly mixing 4.5mmol of Se powder with 2.5mL of octylamine and 2.5mL of oleylamine in a second mixed solvent at room temperature to obtain Se precursor solution;
and step three, adding the Se precursor solution in the step two into the reaction solution in the step one, heating to 95 ℃, reacting for 16 hours, cooling to room temperature, washing the obtained precipitate with a chloroform solution for 3 times, uniformly mixing the precipitate with 30mL of 0.1mol/L cetyltrimethylammonium bromide solution, performing ultrasonic treatment for 60 minutes, washing the precipitate with ethanol for multiple times, and performing vacuum drying at 60 ℃ to obtain the Ag doped CdSe nano-sheet photocatalytic material (1% Ag-CdSe).
Example 2:
the preparation method of the uranium reduction separated Ag doped CdSe nano sheet photocatalytic material comprises the following steps:
step one, 1.47mmol CdCl 2 ·2.5H 2 O and 0.03mmol AgNO 3 Uniformly mixing the mixed powder of (1) with 5mL of octylamine and 5mL of a first mixed solvent of oleylamine, heating to 120 ℃ for reaction for 2 hours, and naturally cooling to room temperature to obtain a reaction solution;
step two, uniformly mixing 4.5mmol of Se powder with 2.5mL of octylamine and 2.5mL of oleylamine in a second mixed solvent at room temperature to obtain Se precursor solution;
and step three, adding the Se precursor solution in the step two into the reaction solution in the step one, heating to 95 ℃, reacting for 16 hours, cooling to room temperature, washing the obtained precipitate with a chloroform solution for 3 times, uniformly mixing the precipitate with 30mL of 0.1mol/L cetyltrimethylammonium bromide solution, performing ultrasonic treatment for 60 minutes, washing the precipitate with ethanol for multiple times, and performing vacuum drying at 60 ℃ to obtain the Ag doped CdSe nano-sheet photocatalytic material (3% Ag-CdSe).
Example 3:
the preparation method of the uranium reduction separated Ag doped CdSe nano sheet photocatalytic material comprises the following steps:
step one, 1.47mmol CdCl 2 ·2.5H 2 O and 0.03mmol AgNO 3 Uniformly mixing the mixed powder of (1) with 5mL of octylamine and 5mL of a first mixed solvent of oleylamine, heating to 120 ℃ for reaction for 2 hours, and naturally cooling to room temperature to obtain a reaction solution;
step two, uniformly mixing 4.5mmol of Se powder with 2.5mL of octylamine and 2.5mL of oleylamine in a second mixed solvent at room temperature to obtain Se precursor solution;
step three, adding Se precursor solution in the step two into the reaction solution in the step one, heating to 95 ℃, reacting for 16 hours, cooling to room temperature, washing the obtained precipitate with chloroform solution for 3 times, adding the precipitate and 30mL of 0.1mol/L cetyltrimethylammonium bromide solution into a supercritical carbon dioxide reaction device, injecting carbon dioxide into the supercritical carbon dioxide reaction device, stirring for 30 minutes at 38 ℃ and 18MPa, decompressing, and then performing ultrasonic treatment for 30 minutes; and washing the precipitate with ethanol for multiple times, and vacuum drying at 60 ℃ to obtain the Ag doped CdSe nano sheet photocatalytic material (3% Ag-CdSe-1).
Example 4:
the preparation method of the uranium reduction separated Ag doped CdSe nano sheet photocatalytic material comprises the following steps:
step one, 1.47mmol CdCl 2 ·2.5H 2 O and 0.03mmol AgNO 3 Uniformly mixing the mixed powder of (1) with 5mL of octylamine and 5mL of a first mixed solvent of oleylamine, heating to 120 ℃ for reaction for 2 hours, and naturally cooling to room temperature to obtain a reaction solution;
step two, uniformly mixing 4.5mmol of Se powder with 2.5mL of octylamine and 2.5mL of oleylamine in a second mixed solvent at room temperature to obtain Se precursor solution;
step three, adding Se precursor solution in the step two into the reaction solution in the step one, heating to 95 ℃, reacting for 16 hours, cooling to room temperature, washing the obtained precipitate with chloroform solution for 3 times, adding the precipitate and 30mL of 0.1mol/L cetyltrimethylammonium bromide solution into a supercritical carbon dioxide reaction device, injecting carbon dioxide into the supercritical carbon dioxide reaction device, stirring for 30 minutes at 38 ℃ and 18MPa, decompressing, and then performing ultrasonic treatment for 30 minutes; washing the precipitate with ethanol for multiple times, and vacuum drying at 60 ℃ to obtain an Ag doped CdSe nano sheet photocatalytic material, and treating the obtained Ag doped CdSe nano sheet photocatalytic material for 2min by using a low-temperature plasma treatment instrument; obtaining Ag doped CdSe nano sheet photocatalytic material (3% Ag-CdSe-2); the atmosphere of the low-temperature plasma treatment instrument is argon; the frequency of the low-temperature plasma treatment instrument is 45KHz, the power is 60W, and the pressure of the atmosphere is 30Pa;
comparative example 1:
the preparation method of the CdSe nano sheet photocatalytic material comprises the following steps:
step one, 1.5mmol CdCl 2 ·2.5H 2 O with 5mL octylamine and 5mL oleylamineUniformly mixing the first mixed solvent, heating to 120 ℃, reacting for 2 hours, and naturally cooling to room temperature to obtain a reaction solution;
step two, uniformly mixing 4.5mmol of Se powder with 2.5mL of octylamine and 2.5mL of oleylamine in a second mixed solvent at room temperature to obtain Se precursor solution;
and step three, adding the Se precursor solution in the step two into the reaction solution in the step one, heating to 95 ℃, reacting for 16 hours, cooling to room temperature, washing the obtained precipitate with a chloroform solution for 3 times, uniformly mixing the precipitate with 30mL of 0.1mol/L cetyltrimethylammonium bromide solution, performing ultrasonic treatment for 60 minutes, washing the precipitate with ethanol for multiple times, and performing vacuum drying at 60 ℃ to obtain the Ag doped CdSe nano-sheet photocatalytic material (CdSe).
Characterization of the morphology of the 3% ag-CdSe material prepared in comparative example 1, example 2, TEM images showed CdSe (fig. 1 (a)), 3% ag-CdSe (fig. 1 (b)) to be in the form of nanoplatelets (fig. 1). HRTEM images of CdSe,3% ag-CdSe are shown in figure 2. FIG. 2 (a) is a HRTEM image of an original CdSe nanosheet with lattice fringes of different directions, wherein a interplanar spacing of 0.37nm corresponds to the (100) plane of the wurtzite structure and a interplanar spacing of 0.35nm corresponds to the (111) plane of the wurtzite structure. This demonstrates that the original CdSe nanoplatelets are composed of both sphalerite and wurtzite crystal structures. FIG. 2 (b) is an HRTEM image of a 3% Ag-CdSe nanosheet, and it can be clearly seen that only one direction of lattice fringes on the 3% Ag-CdSe nanosheet is a (111) plane with a 0.35nm interplanar spacing, corresponding to the sphalerite structure of the CdSe nanosheet. This suggests that the introduction of Ag into CdSe nanoplatelets causes a change in the crystal structure.
As shown in FIG. 3, the original CdSe nano sheet is a combination of two crystal structures of sphalerite (JCPDS No. 19-0191) and wurtzite (JCPDS No. 08-0459), and as Ag is doped, the wurtzite crystal structure in the CdSe nano sheet becomes smaller, the crystalline structure of the sphalerite is gradually prone to sphalerite, and the crystal structure of the original CdSe nano sheet can be changed by doping a small amount of Ag. This conclusion can also be demonstrated from the raman spectra, as shown in fig. 4, the peaks in the a and B regions both disappeared with increasing Ag incorporation, indicating that Ag incorporation causes a change in chemical bonds and thus a change in CdSe nanoplatelet crystal structure. The FT-IR spectrum of Ag-CdSe is shown in FIG. 5.
FIG. 6 (a) is XPS total spectrum of Ag-CdSe nanoplatelets. FIG. 6 (b) is a Cd3d XPS spectrum of an Ag-CdSe nanosheet. It can be clearly seen that the 3d peak of Cd shifts to low binding energy after Ag is doped with CdSe nanoplatelets, indicating that electrons on Se are partially transferred to Cd after Ag doping. At the same time, the 3d XPS spectrum of Se also shifts to lower binding energy with the doping of Ag, indicating that doping of Ag lowers the electron valence of part of Se (FIG. 6 (c)). FIG. 6 (d) is an Ag 3d XPS spectrum, clearly showing that Ag has been successfully incorporated into CdSe nanoplatelets. In conclusion, we successfully synthesized Ag-doped CdSe nanoplates, and a small amount of Ag incorporation induced a change in the crystal structure of the CdSe nanoplates.
In the photocatalytic reduction of U (VI), the energy required for the photocatalytic reduction of U (VI) to U (IV) is about 4.91V, and generally, the conduction band position of the semiconductor must be higher than 4.91V for the photocatalytic reduction of U (VI) to occur completely, and under such conditions, the generated photo-generated electrons can participate in the photocatalytic reduction of U (VI) after the semiconductor is excited by the light source. Therefore, the change of the energy band structure after Ag doping CdSe nano sheet is analyzed by using the Mott Schottky, the ultraviolet diffuse reflection and the UPS. As shown in fig. 7 (a), the positive slopes of the two straight lines indicate that both CdSe and 3% Ag-CdSe nanoplatelets are n-type semiconductors, and compared with the original CdSe nanoplatelets, the carrier density of the 3% Ag-CdSe nanoplatelets after Ag doping is greater, which indicates that Ag doping can improve the conductivity of CdSe and is more favorable for transfer of photogenerated carriers. FIG. 7 (b) shows the calculated band gap widths of CdSe, 1% Ag-CdSe and 3% Ag-CdSe nano-sheets according to the ultraviolet diffuse reflection data, and it can be seen that the doping of Ag can reduce the band gap width of CdSe nano-sheets, and the narrow band gap structure can increase the light absorption wavelength range, thereby being more beneficial to the generation and transition of photogenerated carriers.
FIGS. 8 (a) and (b) are the valence band spectra of CdSe, 1% Ag-CdSe, and 3% Ag-CdSe nanoplatelets, respectively. From the UPS valence band curve and secondary electron edge curve, a corresponding energy band structure diagram can be obtained (fig. 9). The conduction band positions of CdSe, 1% Ag-CdSe and 3% Ag-CdSe are respectively-4.68 eV, -4.63eV and-4.55 eV, and the difference between the conduction band positions and the conduction band positions is 0.23eV, 0.28eV and 0.36eV respectively from the energy required by theoretical photocatalytic reduction of uranium-4.91 eV. It can be seen that the doping of Ag is accompanied by the reduction of the band gap of the CdSe nano sheet, and the conduction band position is also relatively shifted upwards, so that the photocatalytic reduction of U (VI) is facilitated.
U (VI) adsorption-catalytic reduction experiments are carried out on the Ag doped CdSe nano sheet photocatalytic materials prepared in comparative example 1 and examples 1-4 through uranium reduction separation:
after uranium is reduced by photocatalysis, azo arsine III is mixed with the reacted solution, and UO in the solution is monitored by utilizing ultraviolet visible absorption spectrum with the wavelength of 651.8nm 2 2+ Is a concentration of (3).
Dark conditions: respectively at 20mL UO 2 2+ Solution (C) 0 5mg of sample (uranium reduction separated Ag doped CdSe nanoplatelet photocatalytic material prepared in comparative example 1, examples 1 to 4) was added to =200 mg/L, ph=4, stirred at 600r/min for 120min under dark conditions at room temperature, absorbance of the reacted solution was measured by an ultraviolet spectrophotometer (uv visible absorption spectrum was monitored for UO at different reaction times at a wavelength of 651.8nm 2 2+ Concentration), calculating the efficiency of photocatalytic reduction of uranium; all experiments were performed in triplicate and averaged; wherein the removal rate= (C 0 -C t )/C 0 ×100％，C 0 At an initial concentration of C t Is the concentration after adsorption;
illumination conditions: respectively at 20mL UO 2 2+ Solution (C) 0 5mg of sample (Ag doped CdSe nano-sheet photocatalytic material prepared in comparative example 1 and examples 1 to 4) was added to the sample (pH=4) =200 mg/L, simulated sunlight irradiation (300-W Xe lamp BL-GHX-V with AM1.5G filter) was applied at room temperature, stirring was carried out at 600r/min for 160min, and absorbance of the reacted solution was measured by an ultraviolet spectrophotometer (UO with ultraviolet-visible absorption spectrum monitoring different reaction times at a wavelength of 651.8 nm) 2 2+ Concentration), calculating the efficiency of photocatalytic reduction of uranium; all experiments were performed in triplicate and averaged; wherein the removal rate= (C 0 -C t )/C 0 ×100％，C 0 At an initial concentration of C t Concentration after adsorption；
FIG. 10 is a graph of U (VI) removal in dark reaction of CdSe, 1% Ag-CdSe, 3% Ag-CdSe nanoplatelets; FIG. 11 is a graph showing the removal rate of U (VI) in the photoreaction of CdSe, 1% Ag-CdSe, and 3% Ag-CdSe nanoplatelets, wherein the removal rate of U (VI) is less than 3% for all nanoplatelets when no light is applied, because CdSe nanoplatelets have a small specific surface area and few surface adsorption points, and therefore the adsorption to U (VI) is limited (FIG. 10). In contrast, when light is introduced, the CdSe nano sheet generates photo-generated electrons and holes under the influence of the excitation of a light source, and participates in the photocatalytic reduction of U (VI). As shown in FIG. 11, the removal rate of U (VI) by 3% Ag-CdSe nano-sheets was as high as 95.65%, which is 1.9 and 1.2 times that of CdSe nano-sheets (49.7%) and 1% Ag-CdSe nano-sheets (81.3%), respectively. Wherein, the CdSe nano sheet doped with Ag is more beneficial to the photocatalytic reduction U (VI) reaction due to the change of the crystal structure and the band gap width.
FIG. 12 is a graph of U (VI) removal ratios in dark reactions of 3% Ag-CdSe, 3% Ag-CdSe-1, 3% Ag-CdSe-2 nanoplatelets; FIG. 13 is a graph showing the U (VI) removal rate of 3% Ag-CdSe, 3% Ag-CdSe-1, 3% Ag-CdSe-2 nanosheets under a photoreaction, wherein the reaction between the precipitate and cetyltrimethylammonium bromide solution is carried out in a supercritical reaction device, so that the reaction effect of the precipitate and cetyltrimethylammonium bromide can be remarkably improved, the hydrophilicity of the Ag-doped CdSe nanosheets photocatalytic material separated by uranium reduction can be further improved, and the U (VI) removal can be further improved; in addition, the surface treatment is carried out on the Ag doped CdSe nano sheet catalytic material by low-temperature plasma, so that the hydrophilicity of the Ag doped CdSe nano sheet catalytic material separated by uranium reduction is further improved, and the removal of U (VI) is more remarkably improved.
The solid-to-liquid ratio, the anti-ion interference capability and the pH dependence of the 3% Ag-CdSe nano-sheet were further analyzed. FIG. 14 is a solid to liquid ratio of 3% Ag-CdSe nanoplatelets (20 mL UO 2 2+ Solution C 0 The graph of simulated solar radiation (300-W Xe lamp BL-GHX-V with AM1.5G filter) applied at room temperature, with different amounts of 3% ag-CdSe nanoplatelets added, stirred for 120 min) versus U (VI) removal rate, can be seen as followsWhen the solid-liquid ratio is increased and is 0.25, the removal rate of U (VI) is balanced, which shows that the optimal solid-liquid ratio of 3 percent Ag-CdSe nano-sheet photocatalytic reduction uranium is 0.25. Generally, the photocatalytic reduction method is selective and is mainly directed to ions having reducibility (e.g., U (VI) and U (IV)), so that non-reducing ions (e.g., ca) coexist in the solution 2+ 、K + 、Mg 2+ ) The photocatalytic reduction process is capable of selectively photo-reducing U (VI) to U (IV) without being affected by other ions. FIG. 15 is an anti-ion interference graph of 3% Ag-CdSe nanoplatelets, na coexisting in solution + 、K + 、Sr 2+ 、Zn 2+ 、Mg 2+ 、SO 4 2 -, br-, cl-, and U 6+ When the molar ratio of (1) to (1), the removal rate of the 3% Ag-CdSe nano sheet to U (VI) can be maintained to be about 90% (20 mL UO) 2 2+ Solution C 0 10mg/L, simulated solar radiation (300-W Xe lamp BL-GHX-V with AM1.5G filter), ph=4, 3% ag-CdSe nanoplatelets 5mg, stirring for 120 min) was applied at room temperature; for ions having reducing properties, e.g. Cu 2+ The removal rate of U (VI) by the 3% Ag-CdSe nano sheet is slightly reduced. In addition, the surface electronegativity of the material also affects the removal rate of U (VI), while the surface electronegativity of the material is susceptible to the pH of the solution, thus analyzing the pH dependence of the 3% Ag-CdSe nanoplatelets (FIG. 16) (20 mL UO 2 2+ Solution C 0 Simulated solar irradiation (300-W Xe lamp BL-GHX-V with am1.5g filter) was applied at room temperature, at different pH conditions, 3% ag-CdSe nanoplatelets 5mg, stirred for 120 min); it can be seen that as the pH of the solution increases, the removal rate of the 3% ag-CdSe nanoplatelets to U (VI) shows a tendency of a rising and falling, reaching an extreme point at about ph=4.0; based on the above analysis, the optimal experimental conditions of the 3% ag-CdSe nanoplatelets were found, i.e., the 3% ag-CdSe nanoplatelets had a high selectivity to U (VI) at ph=4.0 and a solid to liquid ratio of 0.25.
In order to study the stability of the product and material generated by the 3% Ag-CdSe nano-sheet after the uranium photocatalytic reduction reaction, the corresponding product was collected and tested by XPS analysis, and the results are shown in FIG. 17. FIG. 17 (a) 3% Ag after photocatalytic reactionU4 f XPS spectrum on CdSe nano sheet, the U4 f XPS spectrum can be divided into two main peaks, one is U4 f at 392.3eV 5/2 Peak, one is U4 f at 381.5eV 5/2 Peaks, U (VI) and U (IV), are present together in each peak. This result demonstrates that after the photocatalytic reaction, both ions U (VI) and U (IV) coexist on the 3% Ag-CdSe nanoplatelets, further demonstrating that the product of the photocatalytic reduction is U (IV). FIGS. 17 (b) - (d) are graphs of Cd3d, se 3d, and Ag 3d XPS of 3% Ag-CdSe nanoplatelets after photocatalytic reaction, respectively (before and after photocatalytic reaction). After the photocatalytic reaction, a new peak appears in the 3d XPS spectrum of Se at 52.3eV, and the peak is shifted to the lower binding energy by about 1.1eV compared with the original peak at 53.4eV, which indicates that Se is slightly oxidized during the photocatalytic reaction, and the Cd3d and Ag 3d peaks still remain unchanged. Therefore, under the illumination condition, the photo-generated electrons generated by the CdSe nano sheet participate in the photo-reduction of U (VI), and the photo-generated holes cause slight oxidation of Se, so that a state with unbalanced surface electronegativity is generated, the adsorption of U (VI) is facilitated, and the photo-reduction of U (VI) into U (VI) is realized under the photocatalysis effect.
Further, as shown in FIG. 18, the valence band edge (FIG. 18 (a)) and secondary electron edge curves (FIG. 18 (b)) of the 3% Ag-CdSe nanoflake UPS before and after the photocatalytic reaction are plotted. It can be clearly seen that after the photocatalytic reaction, the secondary electron edge of the 3% ag-CdSe nanoplatelets has one more peak due to the presence of uranium species, which also laterally demonstrates that the 3% ag-CdSe nanoplatelets successfully achieve photocatalytic reduction of U (VI).
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (8)
1. The preparation method of the uranium reduction separated Ag doped CdSe nano sheet photocatalytic material is characterized by comprising the following steps of:
step one, cdCl 2 •2.5H 2 O and AgNO 3 Uniformly mixing the mixed powder of (1) with a first mixed solvent of octylamine and oleylamine, heating to 115-125 ℃, reacting for 1-3 hours, and naturally cooling to room temperature to obtain a reaction solution;
step two, uniformly mixing Se powder with a second mixed solvent of octylamine and oleylamine at room temperature to obtain Se precursor solution;
step three, adding the Se precursor solution in the step two into the reaction solution in the step one, heating to 90-100 ℃, reacting for 14-18 hours, cooling to room temperature, cleaning the obtained precipitate with a chloroform solution for a plurality of times, adding the precipitate and the hexadecyl trimethyl ammonium bromide solution into a supercritical carbon dioxide reaction device, injecting carbon dioxide into the supercritical carbon dioxide reaction device, stirring for 15-30 minutes at the temperature of 35-40 ℃ and the pressure of 12-18 MPa, decompressing, and then performing ultrasonic treatment for 15-30 minutes; and then washing the precipitate with ethanol for multiple times, and vacuum drying to obtain the Ag doped CdSe nano sheet photocatalytic material.
2. The method for preparing a uranium reduction-separated Ag-doped CdSe nanoplatelet photocatalytic material according to claim 1, wherein in the first step, cdCl 2 •2.5H 2 O and AgNO 3 The molar ratio of the components is 1.4-1.5:0.01-0.035; the volume ratio of the octylamine to the oleylamine is 1:1; the molar volume ratio of the mixed powder to the first mixed solvent is 1.5 mmol/10 mL.
3. The method for preparing the uranium reduction-separated Ag-doped CdSe nanosheet photocatalytic material according to claim 1, wherein in the second step, a molar volume ratio of Se powder to the second mixed solvent is 4.5mmol:5mL; the volume ratio of the octylamine to the oleylamine is 1:1.
4. The method for preparing the uranium reduction-separated Ag-doped CdSe nanosheet photocatalytic material according to claim 1, wherein in the third step, the concentration of the cetyltrimethylammonium bromide solution is 0.05-0.15 mol/L; and in the first step, the molar volume ratio of the mixed powder to the cetyltrimethylammonium bromide solution is 1.5 mmol:25-45 mL.
5. The method for preparing the uranium reduction-separated Ag-doped CdSe nanoplatelet photocatalytic material according to claim 1, wherein in the third step, the method further includes: and treating the obtained Ag doped CdSe nano sheet photocatalytic material for 1-3 min by using a low-temperature plasma treatment instrument.
6. The method for preparing the uranium reduction-separated Ag-doped CdSe nanosheet photocatalytic material according to claim 5, wherein the atmosphere of the low-temperature plasma processor is argon; the frequency of the low-temperature plasma treatment instrument is 35-45 KHz, the power is 45-60W, and the pressure of atmosphere is 30-45 Pa.
7. An application of the uranium reduction-separated Ag-doped CdSe nanosheet photocatalytic material prepared by the preparation method according to any one of claims 1-6 in radioactive wastewater treatment, wherein the radioactive wastewater is uranium-containing radioactive wastewater.
8. The application of claim 7, wherein the Ag doped CdSe nano sheet photocatalytic material is added into uranium-containing radioactive wastewater, and the photocatalytic reaction is carried out under the condition that a xenon lamp simulates sunlight, so that the photocatalytic reduction of hexavalent uranium in the uranium-containing radioactive wastewater is realized; at the same time, after the photocatalytic material after the photocatalytic reaction is oxidized in the air again by 48 and h, the photocatalytic material is dispersed to 0.1mol/L KHCO 3 Elution reaction is carried out in solution to remove UO deposited on the catalyst 2 And then washing with water, and drying the collected photocatalyst material for recycling.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009161372A (en) * | 2007-12-28 | 2009-07-23 | Natl Inst Of Radiological Sciences | CdSe QUANTUM DOT AND MANUFACTURING METHOD THEREOF |
| CN104549374A (en) * | 2014-12-16 | 2015-04-29 | 中国科学院理化技术研究所 | Cadmium selenide flower-like microsphere with hydrophilic surface and composed of nanosheets as well as preparation method and application of cadmium selenide flower-like microsphere |
| CN105800570A (en) * | 2016-02-29 | 2016-07-27 | 北京师范大学 | Controllable synthetic method of two-dimensional wurtzite-form cadmium selenide nanomaterials |
| CN106391060A (en) * | 2016-09-07 | 2017-02-15 | 江苏大学 | Preparation method and use of Ag@CdSe/Al2TiO5 composite photocatalyst |
| CN107754822A (en) * | 2017-10-27 | 2018-03-06 | 江苏大学 | A kind of preparation and its application based on CdSe/BiOCl composite photo-catalysts |
| CN108906102A (en) * | 2018-06-11 | 2018-11-30 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | A method of uranium extraction is carried out using photocatalysis technology under visible light |
| CN112958150A (en) * | 2021-03-05 | 2021-06-15 | 西南科技大学 | Preparation of ethylenediamine-coated cadmium telluride nano-belt photocatalyst and separation method of uranium in radioactive wastewater |
-
2021
- 2021-07-08 CN CN202110775914.5A patent/CN113499790B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009161372A (en) * | 2007-12-28 | 2009-07-23 | Natl Inst Of Radiological Sciences | CdSe QUANTUM DOT AND MANUFACTURING METHOD THEREOF |
| CN104549374A (en) * | 2014-12-16 | 2015-04-29 | 中国科学院理化技术研究所 | Cadmium selenide flower-like microsphere with hydrophilic surface and composed of nanosheets as well as preparation method and application of cadmium selenide flower-like microsphere |
| CN105800570A (en) * | 2016-02-29 | 2016-07-27 | 北京师范大学 | Controllable synthetic method of two-dimensional wurtzite-form cadmium selenide nanomaterials |
| CN106391060A (en) * | 2016-09-07 | 2017-02-15 | 江苏大学 | Preparation method and use of Ag@CdSe/Al2TiO5 composite photocatalyst |
| CN107754822A (en) * | 2017-10-27 | 2018-03-06 | 江苏大学 | A kind of preparation and its application based on CdSe/BiOCl composite photo-catalysts |
| CN108906102A (en) * | 2018-06-11 | 2018-11-30 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | A method of uranium extraction is carried out using photocatalysis technology under visible light |
| CN112958150A (en) * | 2021-03-05 | 2021-06-15 | 西南科技大学 | Preparation of ethylenediamine-coated cadmium telluride nano-belt photocatalyst and separation method of uranium in radioactive wastewater |
Non-Patent Citations (1)
| Title |
|---|
| Ghada El-Barbary et al..Cellulose acetate nanofibers embedded with Ag nanoparticles/CdSe/graphene oxide composite for degradation of methylene blue.《Synthetic Metals》.2021,第278卷第3页. * |
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