CN114405522A - ZnIn capable of efficiently reducing hexavalent chromium ions2S4/MoSe2Photocatalyst and process for producing the same - Google Patents
ZnIn capable of efficiently reducing hexavalent chromium ions2S4/MoSe2Photocatalyst and process for producing the same Download PDFInfo
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- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title description 6
- 230000008569 process Effects 0.000 title description 6
- 239000011941 photocatalyst Substances 0.000 claims abstract description 48
- 239000011651 chromium Substances 0.000 claims abstract description 35
- 230000009467 reduction Effects 0.000 claims abstract description 25
- 229910001430 chromium ion Inorganic materials 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229910015667 MoO4 Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- VBNIGYNNILMQRE-UHFFFAOYSA-N O.NN.[Se] Chemical compound O.NN.[Se] VBNIGYNNILMQRE-UHFFFAOYSA-N 0.000 claims 2
- 238000002156 mixing Methods 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 238000004064 recycling Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 abstract description 6
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 abstract description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 abstract description 6
- 230000031700 light absorption Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- YYKKIWDAYRDHBY-UHFFFAOYSA-N [In]=S.[Zn] Chemical compound [In]=S.[Zn] YYKKIWDAYRDHBY-UHFFFAOYSA-N 0.000 abstract 1
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000013112 stability test Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000013508 migration Methods 0.000 description 4
- 230000005012 migration Effects 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 3
- 239000011669 selenium Substances 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 239000011684 sodium molybdate Substances 0.000 description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 2
- 229910016001 MoSe Inorganic materials 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- -1 1, 5-diphenylcarbazone acetone Chemical compound 0.000 description 1
- PSCMQHVBLHHWTO-UHFFFAOYSA-K Indium trichloride Inorganic materials Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- MHWZQNGIEIYAQJ-UHFFFAOYSA-N molybdenum diselenide Chemical compound [Se]=[Mo]=[Se] MHWZQNGIEIYAQJ-UHFFFAOYSA-N 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- UDWJTDBVEGNWAB-UHFFFAOYSA-N zinc indium(3+) sulfide Chemical compound [S-2].[Zn+2].[In+3] UDWJTDBVEGNWAB-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses ZnIn capable of efficiently reducing hexavalent chromium ions2S4/MoSe2A photocatalyst belongs to the technical field of photocatalysis. The invention takes self-made zinc indium sulfide, sodium molybdate dihydrate and selenium powder dissolved in hydrazine hydrate as raw materials, and prepares ZnIn with two-dimensional/two-dimensional close contact by a one-step hydrothermal method2S4/MoSe2A photocatalyst having excellent visible light absorption properties. Under the condition of light irradiation, the photocatalyst can be used for reducing the concentration to 0.05g/L K within 20 minutes2Cr2O7The hexavalent chromium ions in the solution are completely reduced and are recycled for 4 times continuouslyThe reduction rate of hexavalent chromium ions can still reach 100 percent within 25 minutes.
Description
Technical Field
The invention relates to the technical field of photocatalysis, in particular to ZnIn capable of efficiently reducing hexavalent chromium ions2S4/MoSe2A photocatalyst.
Background
With the development of human economy and civilization, heavy metal pair ecologyThe environmental pollution is becoming more and more serious. Among the heavy metals, the hexavalent chromium ion Cr (vi) is one of the most common and dangerous pollutants, on one hand because of its wide application range and on the other hand because of its high water solubility, it is easy to enter the ecosystem by "industrial three wastes". The development of the photocatalytic technology provides a new solution for the elimination of Cr (VI). In the process of photocatalytic reaction, the photocatalyst generates photoproduction electrons with reducibility under the irradiation of sunlight, can directly reduce toxic Cr (VI) into nontoxic Cr (III), and is a safe, economic and green Cr (VI) treatment technology. TiO 22Has the advantages of durability, low cost, low toxicity and good chemical and photophysical stability, and is a common photocatalyst. However, because of its wide band gap, it can only absorb ultraviolet light, which is a relatively small amount of the solar spectrum, and therefore, it is not an ideal material for photocatalytic reduction of Cr (vi). The development of a novel high-efficiency photocatalyst with good visible light responsiveness and high-efficiency Cr (VI) reduction performance is of great significance.
Ternary metal sulfide semiconductor indium zinc sulfide (ZnIn)2S4) Is a direct band gap semiconductor, the band gap of which is about 2.06-2.85 eV (Chai B, Peng T, Zeng P, et al. journal of Physical Chemistry C,2011,115(13):6149 and 6155), and can respond to visible light. In addition, compared with common cadmium sulfide photocatalyst, ZnIn2S4The photocatalyst has less harm to human bodies and environment, has better light stability than cadmium sulfide, and is a photocatalytic material with wide application prospect. However, ZnIn despite the above advantages2S4The photocatalyst still has some defects which are mainly represented by low light absorption capacity, low separation efficiency of photon-generated carriers and slow migration process of photon-generated electrons, and the defects cause single ZnIn2S4The applications in the field of photocatalysis are limited. To increase ZnIn2S4Photocatalytic performance of (1), researchers are on ZnIn2S4Numerous attempts to modify have been made. ZnIn is mixed with a solvent2S4The heterojunction compositely constructed with other narrow bandgap semiconductors is an effective means for improving the photocatalytic performance thereofOne, the first step. By constructing a heterojunction, not only can ZnIn be formed2S4The light absorption range of the optical crystal is expanded, and due to different energy level structures among the component materials, the separation and migration efficiency of photon-generated carriers can be remarkably promoted, so that the ZnIn can be remarkably improved2S4The photocatalytic performance of (a). For example, Jianmei Lu et al convert ZnIn2S4And Co9S8Preparing Co in a compounding way9S8/ZnIn2S4Which can completely reduce Cr (VI) within 45 minutes under the irradiation of visible light (Zhang G, Chen D, Li N, et al, Angewandte chemical International Edition,2020,59(21): 8255-8261.). The preparation of ZnIn by Dongyun Chen et al2S4CdS composite photocatalyst, which has a reduction rate of 100% to Cr (VI) with a concentration of 50mg/L within 40 minutes (Zhang G, Chen D, Li N, et al applied Catalysis B: Environmental 2018,232: 164-174).
Molybdenum diselenide (MoSe)2) Is a two-dimensional semiconductor material with excellent photoelectric property and ZnIn which is a two-dimensional material2S4The two-dimensional/two-dimensional heterojunction interface can provide a large contact surface area, more charge transfer channels and shorter charge transfer distance, thereby being beneficial to the migration and separation of photon-generated carriers. Further, MoSe2The conduction and valence band potentials of (1) are at-0.5 and 1.39eV, respectively, and ZnIn2S4The conduction and valence band potentials of (1) and (0) 99eV, respectively, due to MoSe2Has a conduction band close to ZnIn2S4Thus, when the two are compounded by adopting a proper process, under the excitation of light, MoSe2The photo-generated electrons on the conduction band will rapidly migrate to ZnIn according to the Z-shaped mechanism2S4The valence band of (1) and the photogenerated holes are recombined, so that ZnIn2S4The photo-generated electrons with high reduction capacity on the conduction band will be retained, thereby facilitating the reduction of Cr (vi).
In summary, the invention uses ZnIn2S4Photocatalyst-based by in situ growth of MoSe thereon2Preparation of ZnIn2S4/MoSe2The photocatalyst can efficiently carry out photocatalytic reduction on Cr (VI), and shows a larger practical application prospect.
Disclosure of Invention
The invention aims to provide ZnIn capable of efficiently reducing hexavalent chromium ions2S4/MoSe2Photocatalyst, ZnIn prepared thereby2S4/MoSe2The photocatalyst shows excellent performance and stability of photocatalytic reduction of hexavalent chromium ions, and has the advantages of wide and cheap sources of preparation raw materials, simple and controllable preparation process, easy operation, small harm to the environment and human bodies, and larger practical application prospect.
The purpose of the invention is realized by the following technical scheme:
(1) with Zn (CH)3COO)2·2H2O、InCl3And CH3CSNH2Reacting the raw materials at 180 ℃ for 18 hours by a hydrothermal method, naturally cooling to room temperature after the reaction is finished, then centrifugally separating the precipitate, washing with deionized water and ethanol, and finally drying in vacuum at 60 ℃ to obtain ZnIn2S4。
(2) Self-made ZnIn2S4Ultrasonically dispersing to contain Na2MoO4·2H2O in deionized water, then, a selenium solution dissolved in hydrazine hydrate was dropped into the above dispersion, and stirred for 30 minutes. And finally, transferring the mixed solution into a reaction kettle, preserving heat for 1-3 hours at 180-200 ℃, naturally cooling to room temperature after the reaction is finished, centrifugally separating and precipitating, washing with deionized water and absolute ethyl alcohol in sequence, and finally drying at 60 ℃ under a vacuum condition to obtain the ZnIn2S4/MoSe2A photocatalyst.
Drawings
FIG. 1 is the ZnIn prepared in example 12S4/MoSe2Transmission and high resolution transmission electron micrographs of the photocatalyst;
FIG. 2 is the ZnIn prepared in example 12S4/MoSe2Ultraviolet-visible absorption spectrum of the photocatalyst;
FIG. 3 is the ZnIn prepared in example 12S4/MoSe2A performance diagram of the reduction Cr (VI) of the photocatalyst;
FIG. 4 is the ZnIn prepared in example 12S4/MoSe2A reduction Cr (VI) cycle stability test chart of the photocatalyst;
FIG. 5 is the ZnIn prepared in example 22S4/MoSe2A performance diagram of the reduction Cr (VI) of the photocatalyst;
FIG. 6 is the ZnIn prepared in example 22S4/MoSe2A reduction Cr (VI) cycle stability test chart of the photocatalyst;
Detailed Description
The present invention will be described in detail below with reference to the drawings and specific embodiments, which are only examples and do not limit the scope of the present invention in any way.
Example 1
(1)ZnIn2S4/MoSe2Preparation of the photocatalyst
Weighing 100mg of self-made ZnIn2S420mL of a solution containing 0.0010g of Na was added2MoO4·2H2And O in deionized water, and carrying out ultrasonic treatment for 1 hour. Then, 0.0006g of selenium powder is weighed and added into 2.5mL of hydrazine hydrate, and the mixture is dissolved in 80 ℃ water bath with stirring. Finally, the selenium solution dissolved in hydrazine hydrate is dropped into ZnIn2S4With Na2MoO4·2H2Stirring the mixed dispersion liquid of O for 30 minutes, transferring the mixed liquid into a 50mL reaction kettle, reacting in an oven at 180 ℃ for 3 hours, and naturally cooling to room temperature after the reaction is finished. The obtained product is collected by a centrifugal mode, washed by deionized water and absolute ethyl alcohol in sequence and dried under the vacuum condition of 60 ℃ to obtain ZnIn2S4/MoSe2A photocatalyst. The transmission and high resolution transmission electron microscope photo is shown in figure 1 in the attached drawing of the specification. As can be seen from FIG. 1(a), ZnIn was produced2S4/MoSe2The photocatalyst presents a stacked nanosheet structure. From the high resolution transmission electron microscope of FIG. 1(b), two lattice fringes with different interplanar spacings of 0.32Lattice fringes of nm correspond to ZnIn2S4The (102) crystal plane of (1), the lattice fringes with interplanar spacing of 0.24nm corresponding to MoSe2The (103) plane of (1), and this result confirmed ZnIn2S4/MoSe2Successful preparation of heterojunction photocatalysts, and ZnIn2S4And MoSe2Have close two-dimentional/two-dimentional interface contact between them, help the migration and separation of the charge carrier of photogeneration. The ultraviolet-visible absorption spectrum of the ZnIn is shown in the attached figure 2 of the specification, and the ZnIn can be seen from the figure2S4/MoSe2The absorption edge of the heterojunction photocatalyst is positioned around 600nm, which shows that the heterojunction photocatalyst has excellent visible light response capability.
(2)ZnIn2S4/MoSe2Reduction Cr (VI) performance test of photocatalyst
First, 6 quartz tubes each having a volume of 50mL were taken, and 5mg of the prepared ZnIn was added to each quartz tube2S4/MoSe2Photocatalyst, 20mL of K with a concentration of 0.05g/L was added2Cr2O7Water solution, ultrasonic treatment for 30 minutes; the quartz tube was placed in a photocatalytic reactor and stirred in the dark for 30 minutes to reach equilibrium of adsorption and desorption. Thereafter, the light source (300W Xe lamp) was turned on, 5mL of the reaction solution was taken out of the quartz tube in order every 5 minutes, the reaction solution taken out was centrifuged, and 7mL of 0.2M H was added to 2mL of the supernatant2SO4After the mixture was mixed well, 200. mu.L of 1mM 1, 5-diphenylcarbazone acetone solution was added, and the mixture was shaken for 15 minutes to sufficiently perform the color reaction. And finally, testing the absorbance of the solution by using an ultraviolet-visible spectrophotometer, and analyzing the reduction rate of Cr (VI). The ZnIn2S4/MoSe2The Cr (VI) reduction performance diagram of the photocatalyst is shown in a figure 3 in the figure of the specification. As can be seen from the figure, the reduction rate of the photocatalyst to Cr (VI) reaches 100 percent after 20 minutes of illumination.
(3)ZnIn2S4/MoSe2Reduction Cr (VI) cycle stability test of photocatalyst
ZnIn subjected to sequential photocatalytic reaction in the step (2)2S4/MoSe2The photocatalyst is centrifugally separated and usedWashing with deionized water and ethanol, vacuum drying, and re-dispersing to new K with concentration of 0.05g/L2Cr2O7And (3) in an aqueous solution, and performing a photocatalytic reduction Cr (VI) performance test according to the same flow in the step (2). The above process was repeated 3 times to obtain ZnIn as shown in FIG. 4 of the drawings of the specification2S4/MoSe2And (3) a reduction Cr (VI) cycle stability test chart of the photocatalyst. As can be seen from FIG. 4, after 4 cycles of continuous use, the reduction rate of the photocatalyst to Cr (VI) can still reach 100% within 25 minutes, indicating that the photocatalyst has good cycle stability.
Example 2
(1)ZnIn2S4/MoSe2Preparation of the photocatalyst
Weighing 100mg of self-made ZnIn2S420mL of a solution containing 0.0019g of Na was added2MoO4·2H2And O in deionized water, and carrying out ultrasonic treatment for 1 hour. Then, 0.0012g of selenium powder is weighed and added into 2.5mL of hydrazine hydrate, and the mixture is stirred and dissolved in water bath at 80 ℃. Finally, the selenium solution dissolved in hydrazine hydrate is dropped into ZnIn2S4With Na2MoO4·2H2O for 30 minutes, and then the mixture was transferred to a 50mL reaction vessel and reacted in an oven at 200 ℃ for 1 hour. Naturally cooling to room temperature after the reaction is finished, collecting the obtained product in a centrifugal mode, washing the product by deionized water and absolute ethyl alcohol in sequence, and drying the product under the vacuum condition of 60 ℃ to obtain ZnIn2S4/MoSe2A photocatalyst.
(2)ZnIn2S4/MoSe2Reduction Cr (VI) performance test of photocatalyst
The performance test of photocatalytic reduction of Cr (VI) is carried out according to the step (2) in the example 1, and the performance chart of the obtained reduced Cr (VI) is shown in the attached figure 5 in the specification. As can be seen from FIG. 5, the photocatalyst achieved 100% reduction of Cr (VI) in 20 minutes.
(3)ZnIn2S4/MoSe2Cr (VI) reduction cycle stability test of photocatalyst
The photocatalytic Cr (VI) reduction cycle stability test is carried out according to the step (3) in the example 1, and the obtained Cr (VI) reduction cycle stability test chart is shown in the attached figure 6 of the specification. As can be seen from FIG. 6, after 4 continuous cycles, the reduction rate of Cr (VI) by the photocatalyst can still reach 100% within 25 minutes.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (3)
1. ZnIn capable of efficiently reducing hexavalent chromium ions2S4/MoSe2A photocatalyst, characterized in that the ZnIn2S4/MoSe2The photocatalyst can be used for reducing the concentration of 0.05g/L K in 20 minutes2Cr2O7The hexavalent chromium ions in the aqueous solution are completely reduced, and after continuous 4 times of recycling, the reduction rate of the hexavalent chromium ions in 25 minutes can still reach 100 percent, and the preparation method comprises the following steps: self-made ZnIn2S4Ultrasonically dispersing to Na with the concentration of 0.05-0.1 g/L2MoO4·2H2Adding 0.24-0.48 g/L hydrazine hydrate selenium solution into O aqueous solution, dripping the hydrazine hydrate selenium solution into the dispersion liquid, stirring, mixing, transferring into a hydrothermal reaction kettle for hydrothermal reaction, cooling, centrifuging, washing and drying the product in vacuum after the reaction is finished to obtain ZnIn2S4/MoSe2A photocatalyst.
2. The ZnIn capable of efficiently reducing hexavalent chromium ions according to claim 12S4/MoSe2The photocatalyst is characterized in that the hydrothermal reaction temperature is 180-200 ℃, and the hydrothermal reaction time is 1-3 hours.
3. The ZnIn capable of efficiently reducing hexavalent chromium ions according to claim 12S4/MoSe2Photocatalyst, characterized in that, MoSe2And ZnIn2S4The mass ratio of (A) to (B) is 1-2: 100.
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| CN202210094250.0A CN114405522A (en) | 2022-03-30 | 2022-03-30 | ZnIn capable of efficiently reducing hexavalent chromium ions2S4/MoSe2Photocatalyst and process for producing the same |
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| CN202210094250.0A CN114405522A (en) | 2022-03-30 | 2022-03-30 | ZnIn capable of efficiently reducing hexavalent chromium ions2S4/MoSe2Photocatalyst and process for producing the same |
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| CN115072855A (en) * | 2022-07-20 | 2022-09-20 | 常州大学 | Method for reducing hexavalent chromium in wastewater by piezoelectric catalysis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115072855A (en) * | 2022-07-20 | 2022-09-20 | 常州大学 | Method for reducing hexavalent chromium in wastewater by piezoelectric catalysis |
| CN115072855B (en) * | 2022-07-20 | 2023-10-20 | 常州大学 | Method for piezoelectricity catalytic reduction of hexavalent chromium in wastewater |
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