CN115212909A - Cauliflower-shaped CdS/C 3 N 4 Hydrothermal synthesis method and application of composite material - Google Patents
Cauliflower-shaped CdS/C 3 N 4 Hydrothermal synthesis method and application of composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 32
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 18
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 13
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 13
- 150000001661 cadmium Chemical class 0.000 claims abstract description 12
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 12
- JZRWCGZRTZMZEH-UHFFFAOYSA-N thiamine Chemical compound CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N JZRWCGZRTZMZEH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 5
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 11
- 229930003270 Vitamin B Natural products 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 235000019156 vitamin B Nutrition 0.000 claims description 9
- 239000011720 vitamin B Substances 0.000 claims description 9
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 8
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 8
- 239000011941 photocatalyst Substances 0.000 claims description 6
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 3
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims description 3
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 9
- 239000011593 sulfur Substances 0.000 abstract description 8
- 229910052717 sulfur Inorganic materials 0.000 abstract description 8
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 29
- 239000011651 chromium Substances 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 238000007789 sealing Methods 0.000 description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 6
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- QCQCHGYLTSGIGX-GHXANHINSA-N 4-[[(3ar,5ar,5br,7ar,9s,11ar,11br,13as)-5a,5b,8,8,11a-pentamethyl-3a-[(5-methylpyridine-3-carbonyl)amino]-2-oxo-1-propan-2-yl-4,5,6,7,7a,9,10,11,11b,12,13,13a-dodecahydro-3h-cyclopenta[a]chrysen-9-yl]oxy]-2,2-dimethyl-4-oxobutanoic acid Chemical compound N([C@@]12CC[C@@]3(C)[C@]4(C)CC[C@H]5C(C)(C)[C@@H](OC(=O)CC(C)(C)C(O)=O)CC[C@]5(C)[C@H]4CC[C@@H]3C1=C(C(C2)=O)C(C)C)C(=O)C1=CN=CC(C)=C1 QCQCHGYLTSGIGX-GHXANHINSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
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- 238000002360 preparation method Methods 0.000 description 2
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- 238000006557 surface reaction Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- BFGKITSFLPAWGI-UHFFFAOYSA-N chromium(3+) Chemical compound [Cr+3] BFGKITSFLPAWGI-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
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- 238000004043 dyeing Methods 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite nitride Chemical class 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
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- 238000005067 remediation Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Classifications
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- B01J35/39—
-
- 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
- B01J27/24—Nitrogen compounds
-
- 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—
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- 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 cauliflower-shaped CdS/C 3 N 4 The hydrothermal synthesis method of the composite material and the application thereof comprise the following steps: (1) G to C 3 N 4 Adding soluble cadmium salt into water, and performing ultrasonic crushing to obtain a mixed solution A; vitamin B 1 Dissolving hydrochloride and hexamethylenetetramine in water to obtain a solution B, and then adding the solution B into the solution A under stirring to obtain a mixed solution C; (3) Carrying out hydrothermal treatment on the mixed solution C to obtain cauliflower-shaped CdS/C 3 N 4 A composite material. The invention uses vitamin B 1 The hydrochloride is used as a sulfur source and a surfactant to enable CdS to form cauliflower-shaped nanoparticles with smaller sizes, which is beneficial to g-C 3 N 4 And the S-scheme heterojunction is constructed by compounding with CdS, so that the separation of photogenerated electrons and holes is promoted, the utilization rate of visible light is improved, and Cr (VI) can be efficiently catalytically reduced under the condition of visible light, so that the concentration of Cr (VI) is reduced to be below 0.5 mg/L.
Description
Technical Field
The invention belongs to the technical field of material preparation and environmental protection, and particularly relates to cauliflower-shaped CdS/C 3 N 4 A hydrothermal synthesis method of the composite material and application thereof in visible light catalytic reduction of potassium dichromate.
Background
Chromium is a common heavy metal pollutant in industrial wastewater of electroplating, metallurgy, printing and dyeing and the like, and the main existing forms of chromium in nature comprise two oxidation states of chromium (VI) and chromium (III). Among them, too high Cr (VI) concentration is toxic to most organisms, carcinogenic to animals and humans, and causes irritation, and can be enriched by bio-chain action. Therefore, before the chromium (VI) -containing wastewater is discharged into the environment, cr (VI) therein must be removed.
Among the reported methods, the semiconductor-based photocatalytic process for reducing hexavalent chromium to trivalent chromium has been the focus of much research. The photocatalytic reduction method for reducing hexavalent chromium is one of the strategies for effectively repairing polluted wastewater and is one of the first-choice methods for reducing hexavalent chromium due to high efficiency, environmental protection and low cost.
Many photocatalysts have been developed for the remediation of environmental pollutants emitted industrially, such as titanium dioxide, bismuth sulfide, zinc oxide, graphite nitride, and cadmium sulfide. CdS was introduced as a suitable visible light driven photocatalyst because its band gap is relatively narrow, about 2.4eV, and the appropriate band edge position corresponds well to the solar spectrum. However, the rapid recombination of electron-hole pairs, photo-erosion and low surface reaction efficiency of CdS materials prevent its application as an effective photocatalyst.
In order to improve the photocatalytic efficiency of CdS nanostructures, several studies have been conducted to control the particle size and morphology of CdS nanostructures, as these parameters directly affect the surface area, light absorption capacity, and carrier kinetics of the catalyst. Nanostructures of CdS currently prepared are diverse, such as nanospheres, nanorods, nanosheets, nanobelts, nanotubes, layered nanostructures, petal-like nanostructures, hollow nanostructures, and the like.
Disclosure of Invention
Aiming at the problems of fast recombination of CdS electron-hole pairs, serious photo-corrosion and low surface reaction efficiency, the invention aims to provide cauliflower-shaped CdS/C 3 N 4 Hydrothermal synthesis of nano composite material with vitamin B 1 Hydrochloride as a sulfur source and surfactant, cd 2+ With vitamin B 1 The hydrochloride salt provides a sulfur source to form CdS and the CdS is reacted with g-C 3 N 4 The heterojunction is constructed by in-situ recombination, after the heterojunction is compounded, cdS forms smaller cauliflower-shaped nanoparticles, the surface area is increased, the separation of photogenerated electrons and cavities is promoted, the utilization rate of visible light is improved, cr (VI) can be efficiently catalytically reduced under the condition of visible light, the concentration of Cr (VI) is reduced to be below 0.5mg/L, and the emission standard is met.
In order to achieve the technical purpose, the invention adopts the technical scheme that:
cauliflower-shaped CdS/C 3 N 4 The hydrothermal synthesis method of the composite material comprises the following steps:
(1) G to C 3 N 4 Adding soluble cadmium salt into water, and performing ultrasonic crushing to obtain a mixed solution A; vitamin B 1 Dissolving hydrochloride and hexamethylenetetramine in water to obtain a solution B, and then adding the solution B into the solution A under stirring to obtain a mixed solution C;
(2) Carrying out hydrothermal treatment on the mixed solution C, and carrying out solid-liquid separation, washing and drying to obtain the CdS/C 3 N 4 A composite material.
G to C of the invention 3 N 4 Can pass through the existingPrepared by a conventional method, for example, one or more of urea, melamine and thiourea are used as precursors and calcined to obtain g-C 3 N 4 And will not be described in detail herein.
Preferably, in the step (1), the soluble cadmium salt is selected from one or more of cadmium nitrate, cadmium sulfate and cadmium acetate.
Preferably, in step (1), the soluble cadmium salt is reacted with g-C 3 N 4 1-10 by mass.
Preferably, in the step (1), the concentration of the soluble cadmium salt in the mixed solution a is 0.02 to 0.2mol/L.
Preferably, in step (1), the soluble cadmium salt and vitamin B 1 The molar ratio of the hydrochloride to the hexamethylenetetramine is 1-5.
Preferably, in the step (1), the vitamin B is contained in the mixed solution B 1 The concentration of the hydrochloride is 0.1-0.3 mol/L.
Preferably, in the step (2), the temperature of the hydrothermal treatment is 100-180 ℃ and the time is 1-24 h.
The invention also provides the cauliflower-shaped CdS/C 3 N 4 The composite material is applied as a photocatalyst for reducing potassium dichromate under visible light;
the method comprises the following specific steps: at room temperature, adding cauliflower-shaped CdS/C 3 N 4 The composite material is added into water with the concentration of potassium dichromate of 10-250 mg/L and reacts for 0.1-12 h.
Preferably, the cauliflower-shaped CdS/C 3 N 4 The volume ratio of the mass of the composite material to the potassium dichromate solution is 1 mg.
The invention utilizes vitamin B 1 As sulfur source and surfactant, hexamethylenetetramine as cadmium ion complexing agent and alkali promoting vitamin B 1 The hydrochloride decomposes to liberate sulphur in g-C 3 N 4 As a carrier, cd 2+ With vitamin B 1 The hydrochloride salt provides a sulfur source to CdS with g-C 3 N 4 The heterojunction is compositely constructed, so that CdS forms smaller cauliflower-shaped nanoparticles, the surface area is increased, and the photogeneration is promotedAnd the separation of electrons and holes improves the utilization rate of visible light. Under the condition of visible light, cr (VI) can be efficiently catalytically reduced, so that the concentration of the Cr (VI) is reduced to be below 0.5mg/L, and the emission standard is reached.
Compared with the prior art, the invention has the advantages that:
1. vitamin B in the invention 1 The hydrochloride is used as a sulfur source and a surfactant; hexamethylenetetramine is used as cadmium ion complexing agent and alkali-promoted vitamin B 1 The hydrochloride is decomposed to release sulfur, and the sulfur and the soluble cadmium salt are controllably synthesized into CdS.
2. The invention adopts the hydrothermal preparation technology to controllably synthesize CdS/C 3 N 4 The composite material forms a cauliflower-shaped structure, the particle size is obviously reduced, and the precise construction of the efficient visible light photocatalyst is facilitated.
3. CdS/C prepared by the invention 3 N 4 The composite material has a nano-sized structure, and can efficiently reduce Cr (VI) in water under visible light so as to reduce the concentration of the Cr (VI) to below 0.5 mg/L.
Drawings
FIG. 1 is an XRD spectrum of the materials prepared in example 1 and comparative example 1;
FIG. 2 is an SEM photograph of the material prepared in example 1.
Fig. 3 is an SEM image of the material prepared in comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Dissolving 6.9mmol of cadmium nitrate in 50mL of water, and adding 0.2gg-C 3 N 4 Ultrasonically dispersing for 0.5h by a cell crusher to obtain a mixed solution A, and dropwise adding 25mL of a solution containing 7.4mmol of vitamin B into the mixed solution A 1 Uniformly stirring a hydrochloride and a 14mmol aqueous solution B of hexamethylenetetramine, transferring the mixture to a hydrothermal kettle, sealing the hydrothermal kettle, and carrying out hydrothermal treatment at 100 ℃ for 24 hours to obtain a mixtureMixing the solution C, washing and drying the mixed solution C to obtain deep yellow solid CdS/C 3 N 4 A composite material.
Example 2
Dissolving 2.5mmol of cadmium sulfate in 40mL of water, adding 0.1333gg-C 3 N 4 Ultrasonically dispersing for 0.5h by using a cell crusher to obtain a mixed solution A, and dropwise adding 30mL of vitamin B containing 3mmol into the mixed solution A 1 Uniformly stirring a hydrochloride and a 10mmol hexamethylenetetramine water solution B, transferring the mixture to a hydrothermal kettle, sealing the hydrothermal kettle, carrying out hydrothermal treatment at 160 ℃ for 24 hours to obtain a mixed solution C, washing and drying the mixed solution C to obtain deep yellow solid CdS/C 3 N 4 A composite material.
Example 3
Dissolving 2.5mmol of cadmium nitrate in 30mL of water, and adding 0.2gg-C 3 N 4 Ultrasonically dispersing for 0.5h by using a cell crusher to obtain a mixed solution A, and dropwise adding 20mL of vitamin B containing 3mmol into the mixed solution A 1 Uniformly stirring a hydrochloride and a 5mmol hexamethylenetetramine water solution B, transferring the mixture to a hydrothermal kettle, sealing the hydrothermal kettle, carrying out hydrothermal treatment at 160 ℃ for 24 hours to obtain a mixed solution C, washing and drying the mixed solution C to obtain deep yellow solid CdS/C 3 N 4 A composite material.
Example 4
2.5mmol of cadmium nitrate is dissolved in 50mL of water, and 0.2667gg-C is added 3 N 4 Ultrasonically dispersing for 0.5h by using a cell crusher to obtain a mixed solution A, and dropwise adding 30mL of vitamin B containing 3mmol into the mixed solution A 1 Uniformly stirring a hydrochloride and a 5mmol hexamethylenetetramine water solution B, transferring the mixture to a hydrothermal kettle, sealing the hydrothermal kettle, carrying out hydrothermal treatment at 180 ℃ for 1h to obtain a mixed solution C, washing the mixed solution C, and drying to obtain deep yellow solid CdS/C 3 N 4 A composite material.
Comparative example 1
Weighing 6.9mmol of cadmium nitrate, dissolving in 50mL of water, ultrasonically dispersing for 0.5h by a cell crusher, and dropwise adding 25mL of vitamin B containing 7.4mmol 1 Uniformly stirring the hydrochloride and a 14mmol hexamethylenetetramine aqueous solution, transferring the mixture to a hydrothermal kettle, sealing the hydrothermal kettle, carrying out hydrothermal treatment at 100 ℃ for 24 hours, washing and drying to obtain the deep yellow solid CdS.
Comparative example 2
Weighing 15g of urea, adding the urea into a glass dish, sealing tin foil paper, and then placing the sealed tin foil paper into a muffle furnace for heat treatment. Heating to 250 deg.C at a rate of 2 deg.C/min from room temperature, maintaining for 2 hr, heating to 530 deg.C at a rate of 5 deg.C/min, maintaining for 2 hr, cooling to room temperature to obtain light yellow solid, acid washing, water washing to neutrality, and oven drying to obtain light yellow solid g-C 3 N 4 。
Comparative example 3
Weighing 2.5mmol of cadmium nitrate, dissolving in 50mL of water, adding 0.2gg-C 3 N 4 Ultrasonically dispersing for 0.5h by using a cell crusher, dropwise adding 20mL of aqueous solution containing 3mmol of sodium sulfide and 5mmol of hexamethylenetetramine, uniformly stirring, transferring to a hydrothermal kettle, sealing, carrying out hydrothermal treatment at 160 ℃ for 24h, washing, and drying to obtain deep yellow solid CdS/C 3 N 4 A composite material.
Comparative example 4
6.9mmol of cadmium nitrate is dissolved in 50mL of water, and 0.2gg-C is added 3 N 4 Ultrasonically dispersing for 0.5h by a cell crusher to obtain a mixed solution A, and dropwise adding 25mL of a solution containing 7.4mmol of vitamin B into the mixed solution A 1 Uniformly stirring the aqueous solution B of the hydrochloride, transferring the aqueous solution B of the hydrochloride to a hydrothermal kettle, sealing the hydrothermal kettle, carrying out hydrothermal treatment at 100 ℃ for 24 hours to obtain a mixed solution C, washing and drying the mixed solution C to obtain a CdS product which is a light yellow solid C 3 N 4 。
Reduction of potassium dichromate:
at room temperature, 20mg of the materials prepared in examples 1 to 4 and comparative examples 1 to 3 are respectively added into 20mL of potassium dichromate aqueous solution with the concentration of 10 to 250mg/L for light-shielding ultrasonic dispersion for 15min, dark reaction is carried out for 30min, a xenon lamp light source is turned on, the catalyst is removed by filtration after 2h of reaction, the concentration of residual Cr (VI) is detected, and the reduction rate is calculated and shown in Table 1:
TABLE 1 data sheet of potassium dichromate reduction ratio
Claims (9)
1. Cauliflower-shaped CdS/C 3 N 4 The hydrothermal synthesis method of the composite material is characterized by comprising the following steps:
(1) G to C 3 N 4 Adding soluble cadmium salt into water, and performing ultrasonic crushing to obtain a mixed solution A; vitamin B 1 Dissolving hydrochloride and hexamethylenetetramine in water to obtain a solution B, and then adding the solution B into the solution A under stirring to obtain a mixed solution C;
(2) Carrying out hydro-thermal treatment on the mixed solution C, and carrying out solid-liquid separation, washing and drying to obtain the CdS/C 3 N 4 A composite material.
2. The hydrothermal synthesis method according to claim 1, characterized in that: in the step (1), the soluble cadmium salt is selected from one or more of cadmium nitrate, cadmium sulfate and cadmium acetate.
3. The hydrothermal synthesis method according to claim 1, characterized in that: in step (1), the soluble cadmium salt is mixed with g-C 3 N 4 The mass ratio of (A) to (B) is 1-10.
4. The hydrothermal synthesis method according to claim 1, characterized in that: in the step (1), the concentration of the soluble cadmium salt in the mixed solution A is 0.02-0.2 mol/L.
5. The hydrothermal synthesis method according to claim 1, characterized in that: in the step (1), the soluble cadmium salt and the vitamin B 1 The molar ratio of the hydrochloride to the hexamethylenetetramine is 1-5.
6. The hydrothermal synthesis method according to claim 1, characterized in that: in the step (1), vitamin B is contained in the mixed solution B 1 The concentration of the hydrochloride is 0.1-0.3 mol/L.
7. The hydrothermal synthesis method according to claim 1, characterized in that: in the step (2), the temperature of the hydrothermal treatment is 100-180 ℃ and the time is 1-24 h.
8. Cauliflower-like CdS/C synthesized by the hydrothermal synthesis method of any one of claims 1-7 3 N 4 The application of the composite material is characterized in that: the obtained product is used as a photocatalyst for reducing potassium dichromate under visible light;
the method comprises the following specific steps: at room temperature, adding cauliflower-shaped CdS/C 3 N 4 The composite material is added into water with the concentration of potassium dichromate of 10-250 mg/L and reacts for 0.1-12 h.
9. Cauliflower-like CdS/C according to claim 8 3 N 4 The application of the composite material is characterized in that: the cauliflower-shaped CdS/C 3 N 4 The ratio of the mass of the composite material to the volume of the potassium dichromate solution is 1 mg.
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