CN114772644A - Preparation and application of surface oxidized tungsten disulfide nanosheet for treating radioactive wastewater - Google Patents
Preparation and application of surface oxidized tungsten disulfide nanosheet for treating radioactive wastewater Download PDFInfo
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- CN114772644A CN114772644A CN202210310332.4A CN202210310332A CN114772644A CN 114772644 A CN114772644 A CN 114772644A CN 202210310332 A CN202210310332 A CN 202210310332A CN 114772644 A CN114772644 A CN 114772644A
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- radioactive wastewater
- tungsten disulfide
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- oxidized tungsten
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 69
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000002354 radioactive wastewater Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052770 Uranium Inorganic materials 0.000 claims abstract description 20
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
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- 229910052724 xenon Inorganic materials 0.000 claims description 3
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- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
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- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
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- 239000010937 tungsten Substances 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/20—Disposal of liquid waste
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a preparation method and application of a tungsten disulfide nanosheet for treating surface oxidation of radioactive wastewater, wherein the preparation method comprises the following steps: dissolving tungsten hexachloride and sodium dodecyl benzene sulfonate into water, then adding thioacetamide aqueous solution, and uniformly stirring and mixing to obtain a mixed solution; and transferring the mixed solution into a high-pressure reaction kettle with a teflon lining, reacting at 180-200 ℃, filtering, washing and drying to obtain the surface oxidized tungsten disulfide nanosheet for treating the radioactive wastewater. Selection of WS according to the invention2Nanosheet as a material system and surface oxidation introduced into WS2The nano-sheet has higher uranium extraction efficiency, and shows excellent anti-interference ion capacity, high cycle stability and strong irradiation in complex radioactive wastewaterAnd (4) stability.
Description
Technical Field
The invention relates to the field of radioactive wastewater treatment, in particular to preparation and application of a tungsten disulfide nanosheet for treating surface oxidation of radioactive wastewater.
Background
Uranium is one of main pollution elements of radioactive wastewater, has long-term radioactivity and chemical toxicity, is easy to migrate along with the environment, and poses threats to the ecological environment and human health. The high-efficiency extraction of uranium from uranium-containing wastewater becomes an extremely important problem for sustainable development of nuclear energy and environmental protection. The photocatalytic reduction of soluble hexavalent uranium (u (vi)) to insoluble tetravalent uranium (u (iv)) is more attractive for the treatment of uranium-containing wastewater due to its efficient, rapid extraction kinetics and excellent selectivity for non-reducing coexisting ions, compared to traditional separation methods.
In recent years, a variety of two-dimensional semiconductor materials, including TiO2、g-C3N4、WO3And graphene, etc., are considered to be promising candidates for the photocatalytic reduction of uranium due to their large specific surface area and abundant active sites. In two-dimensional semiconductor materials, transition metal oxide and sulfide semiconductors generally have energy band structures suitable for photocatalytic reduction of u (vi), and thus exhibit high photocatalytic reduction efficiency. In addition to the band structure, capture and binding of u (vi) at the semiconductor surface is another important factor affecting u (vi) photoreductivity. However, the lack of U (VI) binding sites on the surface of conventional transition sulfide and oxide semiconductors directly limits the transmission of photoelectrons to U (VI), thereby severely affecting the kinetics of the reduction reaction to U (VI). Therefore, there is a strong need to establish a method for manufacturing semiconductors to improve the kinetics of the catalytic reduction reaction on u (vi).
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing surface-oxidized tungsten disulfide nanoplates for the treatment of radioactive wastewater, comprising the steps of:
dissolving tungsten hexachloride and sodium dodecyl benzene sulfonate into water, then adding a thioacetamide aqueous solution, and uniformly stirring and mixing to obtain a mixed solution;
and step two, transferring the mixed solution into a high-pressure reaction kettle with a teflon lining, reacting at 180-200 ℃, filtering, washing and drying to obtain the surface oxidized tungsten disulfide nanosheet for treating the radioactive wastewater.
Preferably, in the first step, the mass ratio of the tungsten hexachloride to the sodium dodecyl benzene sulfonate is 1.5-2.5: 1; the mass ratio of the tungsten hexachloride to the water is 1: 30-35.
Preferably, in the first step, the mass ratio of thioacetamide to water in the aqueous thioacetamide solution is 1: 15-20; the mass ratio of the tungsten hexachloride to the thioacetamide in the thioacetamide aqueous solution is 1: 1.5-2.5.
Preferably, in the step one, the stirring time is 25-35 min.
Preferably, in the second step, the reaction time is 24 hours at 180-200 ℃.
Preferably, in the second step, adding the dried solid product and absolute ethyl alcohol into a reaction kettle, sealing, heating the sealed reaction kettle to 230-245 ℃, controlling the pressure in the reaction kettle to be 6-8 MPa, keeping the temperature and the pressure for 15-20 min, cooling the sealed reaction kettle in an ice-water bath, taking out the solid product, and drying to obtain the surface oxidized tungsten disulfide nanosheet for treating the radioactive wastewater.
Preferably, the method further comprises the following steps: spreading the dried solid product under an excimer ultraviolet lamp for irradiation to obtain a tungsten disulfide nanosheet for treating surface oxidation of radioactive wastewater; the distance between the dried solid product and the excimer ultraviolet lamp is 1-20 mm; the irradiation power of the excimer ultraviolet lamp is 80-100%, and the irradiation time is 5-25 min.
Preferably, the mass ratio of the dried solid product to the absolute ethyl alcohol is 1: 12-18.
The invention also provides application of the surface oxidized tungsten disulfide nanosheet for treating radioactive wastewater prepared by the preparation method in treating radioactive wastewater, which is characterized in that the surface oxidized tungsten disulfide nanosheet is added into the uranium-containing radioactive wastewater, the uranium-containing radioactive wastewater is stirred for 60min under a dark condition, and then a photocatalytic reaction is carried out under a condition that a xenon lamp simulates sunlight, so that the photocatalytic reduction of hexavalent uranium in the uranium-containing radioactive wastewater is realized.
The invention at least comprises the following beneficial effects: selection of WS according to the invention2Nanosheet as a material system and surface oxidation introduced into WS2The nanosheet has high uranium extraction efficiency, and shows excellent anti-interference ion capacity, high cycle stability and strong irradiation stability in complex radioactive wastewater.
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:
figure 1a is a TEM image of the nanoplatelets prepared in example 1; fig. 1b and 1c are HRTEM images of nanoplates prepared in example 1;
fig. 2a is a TEM image of the nanosheet prepared in comparative example 1; figure 2b is a TEM image of the nanoplatelets prepared in example 2;
fig. 3 is an XRD pattern of nanosheets prepared in accordance with the present invention;
FIG. 4 is a Raman spectrum of a nanoplate prepared according to the present invention;
FIG. 5 is an XPS spectrum of nanoplates prepared in accordance with the present invention;
fig. 6a is a water contact angle image of the nanoplatelets prepared in example 1; fig. 6b is a water contact angle image of the nanoplatelets prepared in example 2; fig. 6c is a water contact angle image of the nanoplatelets prepared according to comparative example 1;
FIG. 7 is an XPS spectrum (S2 p) of nanoplates prepared according to the invention;
FIG. 8 shows the effect of nanosheets prepared according to the present invention on U (VI) removal in the dark;
FIG. 9 shows the effect of nanosheets prepared according to the present invention on U (VI) removal in the dark;
FIG. 10 shows the effect of nanosheets prepared according to the present invention on U (VI) removal under light conditions;
FIG. 11 shows the effect of nanosheets prepared according to the present invention on the removal of U (VI) under illumination conditions;
FIG. 12 shows the effect of nanosheets prepared according to the present invention on U (VI) removal under light conditions;
fig. 13 is a TEM elemental mapping of the nanoplatelets prepared in example 1 after photoreduction of u (vi): (a) STEM, (b) O, (c) S, (d) W, and (e) U.
FIG. 14 is an XPS spectrum of nanoplatelets prepared in accordance with the present invention after photo-reduction of U (VI);
FIG. 15 is an XPS spectrum (U4 f) of a nanosheet prepared according to the present invention after photoreduction of U (VI);
FIG. 16 shows the effect of the nanosheets prepared according to the present invention on photoreduction of U (VI) after gamma irradiation;
figure 17 is the photoreduction u (vi) effect of nanoplates prepared according to the invention in multiple cycles;
fig. 18 is the effect of nanosheets on photoreduction of u (vi) under different pH conditions;
FIG. 19 is a graph of the effect of nanoplatelets on photoreduction of U (VI) at different initial concentrations of U (VI);
FIG. 20 shows the effect of nanosheets on photoreduction of U (VI) under different solid-to-liquid ratios;
figure 21 is a graph of the effect of nanosheets on photoreduction of u (vi) in the presence of interfering ions.
The specific implementation mode is as follows:
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.
Example 1:
a preparation method of surface oxidized tungsten disulfide nanosheets for treating radioactive wastewater comprises the following steps:
step one, dissolving 0.89g of tungsten hexachloride and 0.39g of sodium dodecyl benzene sulfonate into 30mL of distilled water, then adding a thioacetamide aqueous solution (1.71g of thioacetamide is dissolved into 30mL of distilled water), stirring for 30 minutes, and uniformly mixing to obtain a mixed solution;
and step two, transferring the mixed solution into a high-pressure reaction kettle with a teflon lining, reacting for 24 hours at 180 ℃, filtering, washing and drying to obtain the surface oxidized tungsten disulfide nanosheet for treating the radioactive wastewater.
Example 2:
a preparation method of surface oxidized tungsten disulfide nanosheets for treating radioactive wastewater comprises the following steps:
step one, dissolving 0.89g of tungsten hexachloride and 0.39g of sodium dodecyl benzene sulfonate into 30mL of distilled water, then adding a thioacetamide aqueous solution (1.71g of thioacetamide is dissolved into 30mL of distilled water), stirring for 30 minutes, and uniformly mixing to obtain a mixed solution;
and step two, transferring the mixed solution into a high-pressure reaction kettle with a teflon lining, reacting for 24 hours at 200 ℃, filtering, washing and drying to obtain the surface oxidized tungsten disulfide nanosheet for treating the radioactive wastewater.
Example 3:
a preparation method of surface oxidized tungsten disulfide nanosheets for treating radioactive wastewater comprises the following steps:
step one, dissolving 0.89g of tungsten hexachloride and 0.39g of sodium dodecyl benzene sulfonate into 30mL of distilled water, then adding thioacetamide aqueous solution (1.71g of thioacetamide is dissolved into 30mL of distilled water), stirring for 30 minutes, and uniformly mixing to obtain mixed solution;
transferring the mixed solution into a high-pressure reaction kettle with a teflon lining, reacting for 24 hours at 180 ℃, filtering, washing, drying, adding the dried solid product and absolute ethyl alcohol into the reaction kettle, sealing, heating the sealed reaction kettle to 240 ℃, controlling the pressure in the reaction kettle to be 8MPa, keeping the temperature and the pressure for 20 minutes, cooling the sealed reaction kettle in an ice-water bath, taking out the solid product, and drying to obtain tungsten disulfide nanosheets oxidized on the surface for treating radioactive wastewater; the mass ratio of the dried solid product to the absolute ethyl alcohol is 1: 15;
example 4:
a preparation method of surface oxidized tungsten disulfide nanosheets for treating radioactive wastewater comprises the following steps:
step one, dissolving 0.89g of tungsten hexachloride and 0.39g of sodium dodecyl benzene sulfonate into 30mL of distilled water, then adding a thioacetamide aqueous solution (1.71g of thioacetamide is dissolved into 30mL of distilled water), stirring for 30 minutes, and uniformly mixing to obtain a mixed solution;
transferring the mixed solution into a high-pressure reaction kettle with a teflon lining, reacting for 24 hours at 180 ℃, filtering, washing, drying, adding the dried solid product and absolute ethyl alcohol into the reaction kettle, sealing, heating the sealed reaction kettle to 240 ℃, controlling the pressure in the reaction kettle to be 8MPa, keeping the temperature and the pressure for 20 minutes, cooling the sealed reaction kettle in an ice-water bath, taking out the solid product, drying, and spreading the dried solid product under an excimer ultraviolet lamp for irradiation to obtain tungsten disulfide nanosheets subjected to surface oxidation and used for treating radioactive wastewater; the distance between the dried solid product and the excimer ultraviolet lamp is 5 mm; the irradiation power of the excimer ultraviolet lamp is 90%, and the irradiation time is 8 min.
Comparative example 1:
a preparation method of epidisulfide tungsten nanosheets for treating radioactive wastewater comprises the following steps:
step one, dissolving 0.89g of tungsten hexachloride and 0.39g of sodium dodecyl benzene sulfonate into 30mL of distilled water, then adding thioacetamide aqueous solution (1.71g of thioacetamide is dissolved into 30mL of distilled water), stirring for 30 minutes, and uniformly mixing to obtain mixed solution;
and step two, transferring the mixed solution into a high-pressure reaction kettle with a teflon lining, reacting for 24 hours at 240 ℃, filtering, washing and drying to obtain the tungsten disulfide nanosheet for treating the radioactive wastewater.
FIG. 1a is a TEM image of surface-oxidized tungsten disulfide nanoplates prepared in example 1, and FIG. 2a is WS prepared in comparative example 12TEM image of the nanosheets; figure 2b is a TEM image of the surface oxidized tungsten disulfide nanoplates prepared in example 2; example 1 and example 2 prepared surface oxidized tungsten disulfide nanoplates as compared to the original WS2The nanoplatelets have a similar nanoplatelet morphology. HRTEM measurements were performed, using as an example the nanoplatelets prepared in example 1, and as shown in FIG. 1b, the lattice fringes with a interplanar spacing of 0.27nm are attributed to hexagonal WS2The (100) plane of (1). Furthermore, HRTEM images show the presence of amorphous domains, which bring about surface active sites; the distance of the stripes in fig. 1c is between 0.69nm and 1.02nm, most likely the edges. Thus, surface oxidized tungsten disulfide nanoplates with amorphous domains have not only surface active sites, but also edge active sites.
In order to further determine the compositional structure of the prepared samples, XRD and raman characterization were performed. WS prepared in comparative example 1, as shown in FIG. 32Shows characteristic peaks at 14.36 °, 32.77 °, 39.60 °, 49.80 ° and 60.01 °, due to hexagonal WS of (002), (100), (103), (105), and (110) planes2(PDF # 84-1398); surface oxidized tungsten disulfide nanoplates prepared in examples 1 and 2 exhibit similar WS2Characteristic peaks, except for a new broad peak at 23.15 °, which is attributed to monoclinic WO3(PDF # 72-1465). Furthermore, the peak positions of the surface oxidized tungsten disulfide nanoplates prepared in examples 1 and 2 decreased with increasing degree of oxidation, indicating that the increase in lattice spacing was caused by surface oxidation. FIG. 4 shows WS prepared in comparative example 12Surface oxidized tungsten disulfide nanoparticles prepared in examples 1 and 2Raman spectra of the sheet; WS preparation of comparative example 12At 355cm-1And 416cm-1Has two peaks respectively attributed to WS2In-plane E of1 2gVibration and out-of-plane A1gAnd (5) vibrating. The peak positions of the surface oxidized tungsten disulfide nanoplates prepared in examples 1 and 2 were positively shifted with increasing degree of oxidation, indicating that the surface oxidation caused lattice expansion.
FIG. 5 shows XPS spectra for materials prepared in comparative example 1, examples 1 and 2; from the XPS spectra, all samples consisted of W, S and O. Fig. 6a shows the water contact angle of the material prepared in comparative example 1, fig. 6b shows the water contact angle of the material prepared in example 2, and fig. 6c shows the water contact angle of the material prepared in example 1, the water contact angle decreasing from 60.3 ° to 24.1 ° from comparative example 1 to example 2 to example 1, which in turn reveals the presence of amorphous tungsten oxide in the form of a hydroxylated surface. In addition, as shown in FIG. 7, a new peak associated with oxidized S appears in the S2 p spectra of the materials prepared in examples 1 and 2, further confirming oxidized WS2The successful preparation.
The photocatalytic tests were carried out in a 100mL photoreactor cooled by recirculating cooling water (25. + -. 2 ℃). In the catalysis process, 5mg of the prepared photocatalyst (examples 1-4 and comparative example 1) is ultrasonically dispersed into 20mL of solutions (C) containing U (VI) with different concentrationsU(VI)＝8mg L-1、30mg L-1、50mg L-1、100mg L-1And 200mg L-1) And adding Tannic Acid (TA) as sacrificial agent into U (VI) solution with different concentrations at a concentration of 1mg L-1. The pH of the suspension was then adjusted with a negligible volume of 0.1M NaOH and 0.1M HCl solution. Before irradiation, the suspension was stirred in the dark for 60 minutes to ensure adsorption-desorption equilibrium. Then, a 300W xenon lamp with an AM 1.5G filter (BL-GHX-V, China) was used as a light source, and the wavelength of the light source was adjusted by a band pass filter. Over a period of time, UO was measured spectrophotometrically at 651.8nm2 2+The concentration of (2). In addition, the performance of the extraction of u (vi) in an interfering ion-containing solution was evaluated in the same way. At each U (VI) lightAfter catalytic cycling, the photocatalyst was exposed to 0.1M KHCO under ultrasonic conditions3The solution was further treated for 4h, washed 3 times with deionized water and absolute ethanol to remove uranium.
After separating the photocatalyst from the liquid phase, the u (vi) concentration was measured at a wavelength of 651.8nm by arsine III idolite spectrophotometry, and the removal rate was calculated.
FIG. 8 shows the adsorption performance (C) of the nanosheets prepared in comparative example 1, example 2 and example 1 to U (VI) under dark conditionsU(Ⅵ)＝8mg L-1，CTA＝1mg L-1，m/V＝0.25g L-1T293K, pH 4.6). The adsorption capacity of the nanosheets prepared in example 1 was 2.12 times and 1.10 times that of the nanosheets prepared in comparative example 1 and example 2, respectively. This result is attributed to the presence of a hydroxylated surface on the nanoplatelets prepared in example 1, providing abundant adsorption sites to capture UO2 2+. FIG. 9 shows nanosheets prepared in examples 1, 3 and 4 at 8mg L under dark conditions- 1Adsorption Properties (C) for U (VI) in the solution of U (VI)U(Ⅵ)＝8mg L-1，CTA＝1mg L-1，m/V＝0.25g L-1T-293K and pH-4.6), it can be seen that the adsorption effect of the nanosheets prepared in examples 3 and 4 under dark conditions is better than that of the nanosheets prepared in example 1, which illustrates that the adsorption effect under dark conditions can be improved by retreating the prepared tungsten disulfide nanosheets.
FIG. 10 shows the adsorption performance (C) of the nano-sheets prepared in comparative example 1, example 2 and example 1 on U (VI) under simulated sunlight conditionsU(Ⅵ)＝8mg L-1，CTA＝1mg L-1，m/V＝0.25g L-1T293K, pH 4.6). After simulated sunlight is introduced into the reaction system, the U (VI) removal efficiency of all the nanosheets is remarkably improved. The nanosheets prepared in comparative example 1 exhibited a removal efficiency of 51.2% after 20 minutes of irradiation. The removal efficiency of the nano-sheets prepared in example 2 and example 1 is 85.3% and 91.8% in 20 minutes, respectively, and the removal rate of the nano-sheets prepared in example 1 to U (VI) reaches 97.4% in 120 minutes. Drawing (A)The adsorption performance (C) of the nanosheets prepared in examples 3 and 1 to U (VI) under simulated sunlight conditions is given in 11U(Ⅵ)＝8mg L-1，CTA＝1mg L-1，m/V＝0.25g L-1T293K, pH 4.6). The nanosheet prepared in example 3 has significantly higher removal efficiency on U (VI) than the nanosheet prepared in example 1; the absorption performance (C) of the nano sheets prepared in the example 4 and the example 1 to U (VI) under the simulated sunlight condition is shown in the same figure 12U(Ⅵ)＝8mg L-1，CTA＝1mg L-1，m/V＝0.25g L-1T293K, pH 4.6). The nanoplatelets prepared in example 4 also have significantly higher u (vi) removal efficiency than the nanoplatelets prepared in example 1.
Fig. 13 is an elemental mapping analysis of the nanoplates prepared in example 1 after photocatalysis U (vi), as the W, S, O and U elements are clearly observed in elemental mapping, confirming the distribution of U on the nanoplate surface prepared in example 1. Fig. 14 shows XPS measurement spectra of the nanosheets prepared in comparative example 1, example 2 and example 1 after photocatalysis u (vi), and uranium signals can be observed. Figure 15 is the U4 f spectrum of the nanoplatelets after photocatalysis U (vi), the U4 f spectrum deconvoluted into four peaks at 380.0eV, 381.6eV, 390.9eV and 392.4 eV. The peaks for 381.6 and 392.4eV are assigned to u (vi) and the peaks for 380.0eV and 390.9eV are assigned to u (iv), indicating that the nanosheet-adsorbed u (vi) is reduced to u (iv) by a photocatalytic process.
Considering that the radiation stability of semiconductors is a key factor for treating actual radioactive wastewater, the method is to use60The influence of gamma ray irradiation on the removal performance of U (VI) by the surface-oxidized tungsten disulfide nanosheet prepared in example 1 was evaluated under Co gamma ray irradiation, and the total dose range was 50kGy to 500 kGy. As shown in fig. 16, there was no significant decrease in the removal efficiency of the nanoplatelets to u (vi) after irradiation, demonstrating the high radiation stability of the nanoplatelets. Since reusability is another important factor in assessing the utility of photocatalysts, the reusability of the surface-oxidized tungsten disulfide nanoplates prepared in example 1 was assessed by five-cycle reduction of u (vi). As shown in fig. 17, the nanoplatelets remained 8 even after 5 cyclesThe U (VI) removal efficiency of 4.5% indicates that it is highly reusable and therefore potentially applicable to practical photocatalytic reduction U (VI).
To evaluate the removal performance of the surface oxidized tungsten disulfide nanoplates prepared in example 1 under various conditions on u (vi), batch experiments were systematically performed. Considering that the pH of the solution plays a crucial role in the U (VI) photoreduction, at an initial concentration of 8mg L-1The nanoplatelet photocatalytic removal of u (vi) was studied at pH range 2.6 to 9.6. As shown in FIG. 18, when the pH of the solution was 4.6 or more, the removal rate of U (VI) was maintained>96 percent. FIG. 19 shows the effect of initial U (VI) concentration on U (VI) removal efficiency. The initial concentration of the nano-sheets in U (VI) is 8 to 200mg L-1And the initial concentration of U (VI) is 200mg L-1Show high removal efficiency on U (VI). FIG. 20 shows the effect of nanosheet catalyst dosage on U (VI) photocatalytic removal at an initial concentration of 8mg L-1The pH value is 4.6; when the solid-to-liquid ratio (m/V) is from 0.05g L-1Increased to 0.55g L-1When the extraction rate of U (VI) is increased from 60.3 percent to 98.7 percent; the enhanced performance of u (vi) removal is due to an increase in the active sites captured by u (vi).
In addition, the excess interfering ion (C) was investigatedM＝80mg L-1,M＝K+,Ca2+,Na+,Zn2+,Fe3+,Cu2+,VO2+,Pb2+、Br-And HCO3 -) Influence on the removal of U (VI) in industrial wastewater. As shown in FIG. 21, except for Fe3+And Cu2+The presence of excess interfering ions hardly reduced the removal efficiency of the surface-oxidized tungsten disulfide nanoplates prepared in example 1 for U (VI), indicating that the nanoplates are significantly resistant.
While embodiments of the invention have been described above, it is not intended to be limited to the details shown, described and illustrated herein, but is to be accorded the widest scope consistent with the principles and novel features herein disclosed, and to such extent that such modifications are readily available to those skilled in the art, and it is not intended to be limited to the details shown and described herein without departing from the general concept as defined by the appended claims and their equivalents.
Claims (9)
1. A preparation method of surface oxidized tungsten disulfide nanosheets for treating radioactive wastewater is characterized by comprising the following steps:
dissolving tungsten hexachloride and sodium dodecyl benzene sulfonate into water, then adding thioacetamide aqueous solution, and uniformly stirring and mixing to obtain a mixed solution;
and step two, transferring the mixed solution into a high-pressure reaction kettle with a teflon lining, reacting at 180-200 ℃, filtering, washing and drying to obtain the surface oxidized tungsten disulfide nanosheet for treating the radioactive wastewater.
2. The preparation method of surface-oxidized tungsten disulfide nanosheets for treating radioactive wastewater according to claim 1, wherein in step one, the mass ratio of tungsten hexachloride to sodium dodecylbenzenesulfonate is 1.5-2.5: 1; the mass ratio of the tungsten hexachloride to the water is 1: 30-35.
3. The method for preparing surface-oxidized tungsten disulfide nanosheets for treating radioactive wastewater according to claim 1, wherein in step one, the mass ratio of thioacetamide to water in the aqueous thioacetamide solution is 1: 15-20; the mass ratio of the tungsten hexachloride to the thioacetamide in the thioacetamide aqueous solution is 1: 1.5-2.5.
4. The method for preparing surface-oxidized tungsten disulfide nanosheets for treating radioactive wastewater according to claim 1, wherein in step one, the stirring time is 25 to 35 min.
5. The method for preparing surface-oxidized tungsten disulfide nanosheets for treating radioactive wastewater according to claim 1, wherein in step two, the reaction time at 180-200 ℃ is 24 hours.
6. The preparation method of surface oxidized tungsten disulfide nanosheets for treating radioactive wastewater according to claim 1, wherein in the second step, the dried solid product and absolute ethyl alcohol are added into a reaction kettle, the reaction kettle is sealed, the sealed reaction kettle is heated to 230-245 ℃, the pressure in the reaction kettle is controlled to be 6-8 MPa, the temperature and pressure are maintained for 15-20 min, then the sealed reaction kettle is cooled in an ice-water bath, the solid product is taken out, and the solid product is dried to obtain the surface oxidized tungsten disulfide nanosheets for treating radioactive wastewater.
7. The method of preparing surface oxidized tungsten disulfide nanoplates for use in the treatment of radioactive wastewater as in claim 6, further comprising: the dried solid product is spread under an excimer ultraviolet lamp for irradiation, and tungsten disulfide nanosheets for treating surface oxidation of radioactive wastewater are obtained; the distance between the dried solid product and the excimer ultraviolet lamp is 1-20 mm; the irradiation power of the excimer ultraviolet lamp is 80-100%, and the irradiation time is 5-25 min.
8. The preparation method of surface-oxidized tungsten disulfide nanosheets for treating radioactive wastewater according to claim 6, wherein the mass ratio of the dried solid product to absolute ethyl alcohol is 1: 12-18.
9. The application of the surface-oxidized tungsten disulfide nanosheet for treating radioactive wastewater prepared by the preparation method of any one of claims 1 to 8 in treating radioactive wastewater is characterized in that the surface-oxidized tungsten disulfide nanosheet is added into the uranium-containing radioactive wastewater, the uranium-containing radioactive wastewater is stirred for 60min under the dark condition, and then a 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.
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