[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

CN116493031A - Tremella-like Al, N-In 2 S 3 CdS/GO photocatalyst and preparation method thereof - Google Patents

Tremella-like Al, N-In 2 S 3 CdS/GO photocatalyst and preparation method thereof Download PDF

Info

Publication number
CN116493031A
CN116493031A CN202310275866.2A CN202310275866A CN116493031A CN 116493031 A CN116493031 A CN 116493031A CN 202310275866 A CN202310275866 A CN 202310275866A CN 116493031 A CN116493031 A CN 116493031A
Authority
CN
China
Prior art keywords
cds
photocatalyst
tremella
thioacetamide
prepared
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202310275866.2A
Other languages
Chinese (zh)
Inventor
王德宝
吴笑群
荆博洋
孙淑春
宋彩霞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Qingdao University of Science and Technology
Original Assignee
Qingdao University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Qingdao University of Science and Technology filed Critical Qingdao University of Science and Technology
Priority to CN202310275866.2A priority Critical patent/CN116493031A/en
Publication of CN116493031A publication Critical patent/CN116493031A/en
Pending legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24Nitrogen compounds
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/02Sulfur; Selenium; Tellurium; Compounds thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/06Aluminium; Calcium; Magnesium; Compounds thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16Heavy metals; Compounds thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P1/00Disinfectants; Antimicrobial compounds or mixtures thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P3/00Fungicides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/8603Removing sulfur compounds
    • B01D53/8612Hydrogen sulfide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/8668Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/40Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • C01B3/042Decomposition of water
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental Sciences (AREA)
  • Plant Pathology (AREA)
  • Pest Control & Pesticides (AREA)
  • Organic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Inorganic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Health & Medical Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Dentistry (AREA)
  • Materials Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Analytical Chemistry (AREA)
  • Biomedical Technology (AREA)
  • Combustion & Propulsion (AREA)
  • Water Supply & Treatment (AREA)
  • Hydrology & Water Resources (AREA)
  • Toxicology (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses tremella-shaped Al, N-In 2 S 3 A photocatalyst of CdS/GO is prepared from metal chloride and glycol through heating to obtain transparent and uniform liquid, adding thioacetamide, stirring to obtain uniform yellow colloid, transferring the yellow colloid to porcelain boat, coating aluminium foil, putting it In tubular furnace, and thermal decomposition reaction with nitrogen as protecting gas to obtain tremella-like Al, N-In with II-type heterojunction mechanism 2 S 3 The composite catalyst is tremella-shaped multilevel structure microspheres assembled by curved porous nano sheets, so that the catalyst is endowed with more active sites exposed, and has higher charge transfer efficiency and strong redox capacity. The catalyst is obtained through pyrolysis, vulcanization and composite synchronous reaction of a liquid precursor, and the preparation method is low in cost and simple in process. The photocatalyst is used for photocatalytic decomposition of water to produce hydrogen, purifying the environment, photocatalytic degradation of formaldehyde and harmful gases, photocatalytic degradation of organic dyes in wastewater and the like, and has excellent photocatalytic activity and stability.

Description

Tremella-like Al, N-In 2 S 3 CdS/GO photocatalyst and preparation method thereof
Technical Field
The invention belongs to the field of catalysis, and relates to a photocatalyst for new hydrogen energy and environmental purification, in particular to an Al, N-In catalyst 2 S 3 A/CdS/GO photocatalyst and a preparation method thereof, in particular to a method for co-doping In by Al and N 2 S 3 A tremella-shaped multilevel structure photocatalyst assembled by/CdS/GO porous nano-sheets and a preparation method thereof.
Background
The development of semiconductor visible light photocatalysts has been considered as the most promising and effective strategy for solving the problems of environmental pollution and energy shortage. In recent years, metal sulfide semiconductor photocatalysts (e.g., cdS, in 2 S 3 、SnS 2 、Cu 2 S) is receiving a great deal of attention due to good visible light response. However, these sulfide photocatalysts face photogenerated electron-hole pairsThe rapid recombination of the metal-S bond and the metal-S bond results in low photocatalytic efficiency, and the problems of photo corrosion and the like caused by the oxidation of the metal-S bond by the photo-generated holes limit the application of the metal-S bond.
Among the many metal sulfide semiconductor materials, cadmium sulfide (CdS) has been of great interest due to its good visible light response. However, practical use is greatly hindered by the problem of severe photo-generated carrier recombination, easy photo-corrosion when used as a photocatalyst in an aqueous solution, and the like. To enhance photocatalytic activity, various strategies including morphology regulation, elemental doping, defect engineering, and heterojunction construction have been developed.
In recent years, indium sulfide (In 2 S 3 ) As an n-type semiconductor having a band gap of 2.0 to 2.3eV, attention has been paid to its advantages such as good stability and low toxicity. However, in currently being prepared 2 S 3 the/CdS heterojunction photocatalyst has either few adsorption active sites or severe photo-corrosion, or is difficult to construct II-type heterojunction, resulting in low carrier separation efficiency and low reduction-oxidation capability.
Disclosure of Invention
The invention is directed to In prepared In the prior art 2 S 3 The CdS heterojunction photocatalyst has the defects of serious photo-corrosion, few adsorption active sites, low separation efficiency of photo-generated carriers, low reduction and oxidation capability and the like, and provides a method for constructing Al and N co-doped In 2 S 3 Preparation method of/CdS/GO heterojunction photocatalyst. The invention is realized by adopting the following technical scheme:
tremella-like Al, N-In 2 S 3 The CdS/GO photocatalyst and the preparation method thereof are characterized In that the Al, N-In 2 S 3 the/CdS/GO photocatalyst is prepared by co-doping In with Al and N 2 S 3 The CdS heterojunction is compounded with Al, N co-doped Graphene Oxide (GO); the Al, N is co-doped with In 2 S 3 Migration of photogenerated carriers in the/CdS heterojunction follows the type II heterojunction mechanism; the tremella-shaped Al, N-In 2 S 3 The CdS/GO photocatalyst is a tremella-shaped multilevel structure microsphere assembled by curved porous nano sheets, is obtained by pyrolysis, vulcanization and composite synchronous reaction of a liquid precursor,the preparation method specifically comprises the following steps:
(1) Weighing 0.5-10.0g of two-point cadmium chloride pentahydrate, 0.5-10.0g of indium chloride and 1-20ml of ethylene glycol, placing into a small bottle with a cover, and stirring in an oil bath pot at 50-90 ℃ until transparent liquid is formed;
(2) Weighing 0.5-10.0g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 15-60min to obtain uniform yellow colloid;
(3) Transferring the yellow colloid obtained in the step (2) into a porcelain boat, coating aluminum foil, placing in a tube furnace, and adding N 2 Heating to 400-700deg.C at a rate of 1-10deg.C/min under atmosphere, maintaining for 1-6 hr, naturally cooling to room temperature, centrifuging and washing the sample with deionized water and ethanol respectively for three times, and oven drying to obtain tremella-like Al, N-In 2 S 3 a/CdS/GO photocatalyst.
The invention has the advantages that: the preparation method is simple and convenient in process, the pyrolysis, vulcanization and compounding of the precursor are completed in one step, and the obtained catalyst has a tremella-shaped multilevel structure assembled by curved porous nano sheets, so that the adsorption of a target is facilitated; graphene oxide is coated on Al, N-In 2 S 3 The surface of the CdS nano-sheet is beneficial to avoiding photo-corrosion; al and N are co-doped, which is beneficial to enhancing the visible light response range; al, N-In 2 S 3 The CdS/GO heterojunction photocatalyst is a II-type heterojunction mechanism, which is favorable for separating photogenerated electrons and holes; the method is applied to photocatalysis hydrogen evolution, indoor purification, photocatalysis formaldehyde degradation and H 2 S gas removal, organic dye wastewater degradation, inhibition of wall bacteria and mold generation and the like, and has good photocatalytic performance and cycle stability.
Drawings
FIG. 1 shows tremella Al, N-In prepared by the method described In example one 2 S 3 XRD spectra of/CdS/GO photocatalyst.
FIG. 2 shows tremella Al, N-In prepared by the method of example 2 S 3 SEM photographs of different multiples of/CdS/GO photocatalyst.
FIG. 3 shows tremella Al, N-In prepared by the method of example 2 S 3 CdS/GO photocatalystsTEM photographs.
FIG. 4 shows tremella Al, N-In prepared by the method of example 2 S 3 HRTEM photograph of/CdS/GO photocatalyst.
FIG. 5 shows tremella Al, N-In prepared by the method of example 2 S 3 STEM-Mapping photographs of/CdS/GO photocatalyst.
FIG. 6 shows tremella Al, N-In prepared by the method of example 2 S 3 Ultraviolet-visible diffuse reflectance spectra of the/CdS/GO photocatalyst, control one and control two samples.
FIG. 7 shows tremella Al, N-In prepared by the method of example 2 S 3 And (3) a graph of the amount of hydrogen in water decomposed by the CdS/GO photocatalyst and the photocatalysts of the first sample and the second sample.
FIG. 7 shows tremella Al, N-In prepared by the method of example 2 S 3 And (3) a graph of the amount of hydrogen in water decomposed by the CdS/GO photocatalyst and the photocatalysts of the first sample and the second sample.
FIG. 8 shows tremella Al, N-In prepared by the method of example 2 S 3 And (3) a graph of the cycle stability of the water generated by decomposing the CdS/GO photocatalyst.
FIG. 9 shows tremella Al, N-In prepared by the method of example 2 S 3 And (3) a graph of the photocatalytic degradation of formaldehyde by the CdS/GO photocatalyst, and the photocatalyst of the first sample and the second sample of the control example.
Detailed Description
The invention is illustrated in further detail by the following examples:
embodiment one:
(1) Weighing 0.86g of two-point cadmium chloride pentahydrate, 0.70 indium chloride and 1.42ml of ethylene glycol, placing into a small bottle with a cover, and stirring in an oil bath pot at 75 ℃ until a transparent liquid phase is formed;
(2) Weighing 0.85g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 30min to obtain uniform yellow colloid;
(3) Transferring the uniform yellow colloid obtained in the step (2) into a porcelain boat, wrapping with aluminum foil, and placing in a tubeCenter of furnace, at N 2 Heating to 650deg.C at a rate of 5deg.C/min under atmosphere, maintaining for 4 hr, naturally cooling to room temperature, washing the sample with deionized water and ethanol respectively, centrifuging for three times, and oven drying to obtain Tremella-like Al, N-In 2 S 3 a/CdS/GO photocatalyst.
Embodiment two:
(1) 2.74g of cadmium chloride pentahydrate at two points, 0.56g of indium chloride and 1.42ml of ethylene glycol are weighed into a capped vial and stirred in an oil bath at 75 ℃ until a clear liquid phase is formed;
(2) Weighing 0.85g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 30min to obtain uniform yellow colloid;
(3) Transferring the uniform yellow colloid obtained in the step (2) into a porcelain boat, wrapping an aluminum foil, placing the porcelain boat in the center of a tube furnace, and placing the porcelain boat in N 2 Heating to 650deg.C at a rate of 5deg.C/min under atmosphere, maintaining for 4 hr, naturally cooling to room temperature, washing the sample with deionized water and ethanol respectively, centrifuging for three times, and oven drying to obtain Tremella-like Al, N-In 2 S 3 a/CdS/GO photocatalyst.
Embodiment III:
(1) 0.69g of cadmium chloride, 2.23g of indium chloride and 1.42ml of ethylene glycol are weighed into a capped vial and stirred in an oil bath at 75 ℃ until a clear liquid phase is formed;
(2) Weighing 0.85g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 30min to obtain uniform yellow colloid;
(3) Transferring the uniform yellow colloid obtained in the step (2) into a porcelain boat, wrapping an aluminum foil, placing the porcelain boat in the center of a tube furnace, and placing the porcelain boat in N 2 Heating to 650deg.C at a rate of 5deg.C/min under atmosphere, maintaining for 4 hr, naturally cooling to room temperature, washing the sample with deionized water and ethanol respectively, centrifuging for three times, and oven drying to obtain Tremella-like Al, N-In 2 S 3 a/CdS/GO photocatalyst.
Embodiment four:
(1) 0.86g of cadmium chloride pentahydrate at two points, 0.70g of indium chloride and 2.19ml of ethylene glycol are weighed into a capped vial and stirred in an oil bath at 75 ℃ until a transparent liquid phase is formed;
(2) Weighing 1.28g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 30min to obtain uniform yellow colloid;
(3) Transferring the uniform yellow colloid obtained in the step (2) into a porcelain boat, wrapping an aluminum foil, placing the porcelain boat in the center of a tube furnace, and placing the porcelain boat in N 2 Heating to 700 ℃ at a speed of 10 ℃/min under atmosphere, preserving heat for 2 hours, naturally cooling the tube furnace to room temperature, respectively cleaning the sample with deionized water and ethanol, centrifuging for three times, and drying to obtain tremella Al, N-In 2 S 3 a/CdS/GO photocatalyst.
Fifth embodiment:
(1) 1.78g of cadmium chloride pentahydrate at two points, 0.70g of indium chloride and 2.84ml of ethylene glycol are weighed into a capped vial and stirred in an oil bath at 75 ℃ until a clear liquid phase is formed;
(2) Weighing 1.70g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 45min to obtain uniform yellow colloid;
(3) Transferring the uniform yellow colloid obtained in the step (2) into a porcelain boat, wrapping an aluminum foil, placing the porcelain boat in the center of a tube furnace, and placing the porcelain boat in N 2 Heating to 650deg.C at a rate of 2deg.C/min under atmosphere, maintaining for 3 hr, naturally cooling to room temperature, washing the sample with deionized water and ethanol respectively, centrifuging for three times, and oven drying to obtain Tremella-like Al, N-In 2 S 3 a/CdS/GO photocatalyst.
Example six:
(1) 3.56g of cadmium chloride pentahydrate at two points, 0.70g of indium chloride and 4.26ml of ethylene glycol are weighed into a capped vial and stirred in an oil bath at 75 ℃ until a clear liquid phase is formed;
(2) Weighing 2.55g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 30min to obtain uniform yellow colloid;
(3) Transferring the uniform yellow colloid obtained in the step (2) into a porcelain boat, wrapping an aluminum foil, placing the porcelain boat in the center of a tube furnace, and placing the porcelain boat in N 2 Heating to 450 ℃ at a speed of 10 ℃/min under the atmosphere, preserving heat for 6 hours, and naturally cooling the tube furnace to room temperatureRespectively cleaning the sample with deionized water and ethanol, centrifuging for three times, and oven drying to obtain Tremella-like Al, N-In 2 S 3 a/CdS/GO photocatalyst.
Embodiment seven:
(1) 0.86g of cadmium chloride pentahydrate at two points, 2.80g of indium chloride and 4.26ml of ethylene glycol are weighed into a capped vial and stirred in an oil bath at 75 ℃ until a transparent liquid phase is formed;
(2) Weighing 2.55g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 30min to obtain uniform yellow colloid;
(3) Transferring the uniform yellow colloid obtained in the step (2) into a porcelain boat, wrapping an aluminum foil, placing the porcelain boat in the center of a tube furnace, and placing the porcelain boat in N 2 Heating to 700 ℃ at a speed of 2 ℃/min under the atmosphere, preserving heat for 4 hours, naturally cooling the tube furnace to room temperature, respectively cleaning the sample with deionized water and ethanol, centrifuging for three times, and drying to obtain tremella Al, N-In 2 S 3 a/CdS/GO photocatalyst.
Comparative example one:
(1) 1.40 indium chloride and 1.42ml ethylene glycol were weighed into a capped vial and stirred in an oil bath at 75 ℃ until a clear liquid phase formed;
(2) Weighing 0.85g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 30min to obtain uniform yellow colloid;
(3) Transferring the uniform yellow colloid obtained in the step (2) into a porcelain boat, wrapping an aluminum foil, placing the porcelain boat in the center of a tube furnace, and placing the porcelain boat in N 2 Heating to 650deg.C at a rate of 5deg.C/min under atmosphere, maintaining for 4 hr, naturally cooling to room temperature, washing the sample with deionized water and ethanol respectively, centrifuging for three times, and oven drying to obtain Tremella-like Al, N-In 2 S 3 a/CdS/GO photocatalyst.
Control II:
(1) Weighing 0.86g of two-point cadmium chloride pentahydrate and 1.42ml of ethylene glycol, placing into a small bottle with a cover, and stirring in an oil bath pot at 75 ℃ until a transparent liquid phase is formed;
(2) Weighing 0.85g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 30min to obtain uniform yellow colloid;
(3) Transferring the uniform yellow colloid obtained in the step (2) into a porcelain boat, wrapping an aluminum foil, placing the porcelain boat in the center of a tube furnace, and placing the porcelain boat in N 2 Heating to 650deg.C at a rate of 5deg.C/min under atmosphere, maintaining for 4 hr, naturally cooling to room temperature, washing the sample with deionized water and ethanol respectively, centrifuging for three times, and oven drying to obtain Tremella-like Al, N-In 2 S 3 a/CdS/GO photocatalyst.
FIG. 1 shows tremella-like In prepared by the method described In example one 2 S 3 XRD spectra of/CdS/GO. As shown In FIG. 1, according to In 2 S 3 (PDF No. 73-1366) Standard data, in was obtained In comparative example one 2 S 3 Catalyst according to CdS (PDFNo. 41-1049) standard data, a CdS catalyst was obtained in comparative example II. For the example samples, there were distinct characteristic peaks at 24.76 °, 26.52 °, 28.19 °, 43.78 °, 36.58 °, 43.78 °, 43.67 °, 47.79 ° and 51.80 ° corresponding to the (100), (002), (101), (102), (110), (103) and (112) crystal planes of CdS (pdfno. 41-1049). Characteristic peaks at 14.22 °, 23.34 °, 27.36, 43.46 °, and 47.63 ° correspond to In 2 S 3 The (103), (116), (109), (0012), (309) and (316) crystal planes of (PDF No. 73-1366) and according to In 2 S 3 (PDF No. 73-1366) standard data, these diffraction peaks are all shifted to high diffraction angles, because Al, N atoms are significantly smaller In radius than In, S atoms, al, N co-doped In 2 S 3 After that, in is made 2 S 3 The lattice parameter becomes smaller. XRD results show that the invention successfully synthesizes Al and N co-doped In 2 S 3 A CdS heterojunction photocatalyst.
FIG. 2 shows tremella Al, N-In prepared by the method of example 2 S 3 SEM photograph of a/CdS/GO photocatalyst. As shown In FIG. 2, al, N-In 2 S 3 the/CdS/GO sample is tremella-shaped flower ball aggregate with hierarchical structure, each flower has a diameter of about 1-2 μm, and the outer surface shows staggered growth of lamellar curved structure. The nanoplatelets cluster together in different directions to form open cavities distributed over the entire surface of the microsphere. Such an open cavity would resultRich voids and large specific surface area, and exposes more active sites, which is beneficial for photocatalytic reaction.
FIG. 3 shows tremella Al, N-In prepared by the method of example 2 S 3 TEM photograph of a/CdS/GO photocatalyst. As can be seen from fig. 3, the tremella-like flower ball is assembled from ultra-thin nano-sheets, and the light areas along the perimeter indicate that the perimeter of the flower ball is composed of very thin flakes, consistent with SEM images. This unique flower-ball structure imparts Al, N-In 2 S 3 The larger surface area and more reaction sites of the/CdS/GO photocatalyst, the open structure allows electrolyte water molecules to easily enter the interlayer space between ultrathin nanoplatelets.
FIG. 4 shows tremella Al, N-In prepared by the method of example 2 S 3 HRTEM photograph of/CdS/GO photocatalyst. As can be seen from FIG. 4, the enlargement of region 1 In the figure shows two distinct lattice fringes, 0.269nm of which is compared with In 2 S 3 The (00) interplanar spacing of 0.316nm lattice fringes match the (101) interplanar spacing of CdS. At the same time, by enlarging the region 2, it can be seen that there are several almost transparent graphene oxide layers at the catalyst edge, about 0.37nm lattice fringes, matching the interlayer distance of the graphene oxide. The paper can successfully prepare the Al, N-In coated by the graphene oxide shell layer by a liquid precursor assisted one-pot pyrolysis method 2 S 3 a/CdS/GO composite material. The graphene oxide shell can inhibit the photo-corrosiveness of metal sulfide to a certain extent, and accelerate the electron transmission of charges at an interface, so that the photo-catalytic activity and stability are greatly improved. In addition, a tightly coupled interface can be clearly observed, facilitating electron transfer, which provides a good basis for the establishment of a type II heterojunction.
FIG. 5 shows tremella Al, N-In prepared by the method of example 2 S 3 STEM-Mapping photographs of/CdS/GO photocatalyst. As can be seen more clearly from STEM in fig. 5, the tremella-like flower-ball structured catalyst is assembled from ultra-thin nano-sheets. The Mapping pictures of the elements clearly show S, cd, in and C, O,N, al, and the distribution of Cd, in and S elements is tighter than that of C, so that the formation of graphene oxide shells can be verified, and the existence and distribution of Al and N elements can prove the doping of Al and N.
FIG. 6 shows tremella Al, N-In prepared by the method of example 2 S 3 Ultraviolet-visible diffuse reflectance spectra of the/CdS/GO photocatalyst, control one and control two samples. As can be seen more clearly in FIG. 6, the second sample of the control example showed a distinct absorption edge at 520 nm. Whereas the absorption edge of the sample of the control example was approximately 577nm. In contrast, example one Al, N-In 2 S 3 The absorption edge of the/CdS/GO photocatalyst material is at 529nm, the absorption edge of the composite material gradually moves rightwards, namely moves towards the long wave direction, the visible light absorption is obviously enhanced, the utilization efficiency of sunlight is improved, and the high photocatalytic performance is caused.
FIG. 7 shows tremella Al, N-In prepared by the method of example 2 S 3 And (3) a graph of the amount of hydrogen in water decomposed by the CdS/GO photocatalyst and the photocatalysts of the first sample and the second sample. Adopting an on-line photocatalysis system, simulating solar light irradiation by using a xenon lamp (lambda is more than or equal to 420 nm) and using 0.25M Na 2 S/0.35M Na 2 SO 3 As a sacrificial reagent, the photocatalytic activity of the photocatalyst was examined. As shown In FIG. 7, tremella Al, N-In prepared In example I 2 S 3 The hydrogen yield of the/CdS/GO photocatalyst reaches 65.5mmol/g in 6 hours, and the hydrogen evolution rate is 10.9 mmol.g -1 ·h -1 The catalytic performance of the photocatalyst is significantly improved compared with that of the first and second comparative examples. Comparative example A photocatalyst has a hydrogen evolution rate of only 2.6 mmol.g -1 ·h -1 The hydrogen evolution rate of the photocatalyst of comparative example II was 3.7 mmol.g -1 ·h -1 . The obvious improvement of the photocatalysis performance is due to the II-type heterojunction Al, N-In 2 S 3 the/CdS/GO photocatalyst retains holes and electrons having strong oxidation and reduction ability. This high photocatalytic activity is of great importance for the exploitation of hydrogen energy.
FIG. 8 shows tremella Al, N-In prepared by the method of example 2 S 3 And (3) a water hydrogen production amount circulation stability relation graph of the photo-catalytic decomposition of the CdS/GO photocatalyst. As shown In FIG. 8, the process is repeated for 5 times and 6 hours each time, and tremella-like Al, N-In 2 S 3 The hydrogen production performance of the/CdS/GO photocatalyst is not obviously reduced, which indicates that the tremella Al, N-In prepared by the invention 2 S 3 the/CdS/GO photocatalyst has good cycling stability.
FIG. 9 shows tremella Al, N-In prepared by the method of example 2 S 3 And (3) a graph of the photocatalytic degradation of formaldehyde by the CdS/GO photocatalyst, the first catalyst of the control example and the second catalyst of the control example. As can be seen from FIG. 9, tremella-like Al, N-In 2 S 3 The photocatalytic formaldehyde degradation effect of the/CdS/GO photocatalyst is far better than that of the first and second catalyst samples of the comparison example, and the degradation rate of the purified formaldehyde can reach 94% after 60 min. The high photocatalytic activity has important significance for degrading formaldehyde and purifying air.
In addition, the tremella Al, N-In prepared by the method of the invention is simulated by utilizing a xenon lamp (lambda is more than or equal to 420 nm) to irradiate sunlight 2 S 3 The CdS/GO photocatalyst is used for simulating the photocatalytic degradation of wastewater by various organic dyes, and the ultraviolet and visible absorption experimental results of the organic dyes show that various organic dyes can be rapidly degraded under the irradiation of simulated solar light, thus showing that tremella-like Al, N-In prepared by the invention 2 S 3 the/CdS/GO photocatalyst can be used for purifying organic dye wastewater. Tremella Al, N-In prepared by the invention 2 S 3 the/CdS/GO photocatalyst is used for interior wall coating, can avoid the generation of mould In indoor humid environment, and can well remove formaldehyde, ammonia gas and hydrogen sulfide gas In indoor air, so that the tremella Al, N-In prepared by the invention is illustrated 2 S 3 the/CdS/GO photocatalyst can be used in the fields of air purification and environmental purification.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited by the above examples, and any other changes, substitutions, simplifications, etc. made without departing from the principles of the present invention and the technical process are all equivalent substitutions and should be included in the protection scope of the present invention.

Claims (1)

1. Tremella-like Al, N-In 2 S 3 The CdS/GO photocatalyst and the preparation method thereof are characterized In that the Al, N-In 2 S 3 the/CdS/GO photocatalyst is prepared by co-doping In with Al and N 2 S 3 The CdS heterojunction is compounded with Al, N co-doped Graphene Oxide (GO); the Al, N is co-doped with In 2 S 3 Migration of photogenerated carriers in the/CdS heterojunction follows the type II heterojunction mechanism; the tremella-shaped Al, N-In 2 S 3 The CdS/GO photocatalyst is a tremella-shaped multilevel structure microsphere assembled by curved porous nano sheets, and is obtained by pyrolysis, vulcanization and composite synchronous reaction of a liquid precursor, and the preparation method specifically comprises the following steps:
(1) Weighing 0.5-10.0g of two-point cadmium chloride pentahydrate, 0.5-10.0g of indium chloride and 1-20ml of ethylene glycol, placing into a small bottle with a cover, and stirring in an oil bath pot at 50-90 ℃ until transparent liquid is formed;
(2) Weighing 0.5-10.0g of thioacetamide, adding the thioacetamide into the transparent liquid obtained in the step (1), and stirring for 15-60min to obtain uniform yellow colloid;
(3) Transferring the yellow colloid obtained in the step (2) into a porcelain boat, coating aluminum foil, placing in a tube furnace, and adding N 2 Heating to 400-700deg.C at a rate of 1-10deg.C/min under atmosphere, maintaining for 1-6 hr, naturally cooling to room temperature, centrifuging and washing the sample with deionized water and ethanol respectively for three times, and oven drying to obtain tremella-like Al, N-In 2 S 3 a/CdS/GO photocatalyst.
CN202310275866.2A 2023-03-21 2023-03-21 Tremella-like Al, N-In 2 S 3 CdS/GO photocatalyst and preparation method thereof Pending CN116493031A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310275866.2A CN116493031A (en) 2023-03-21 2023-03-21 Tremella-like Al, N-In 2 S 3 CdS/GO photocatalyst and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310275866.2A CN116493031A (en) 2023-03-21 2023-03-21 Tremella-like Al, N-In 2 S 3 CdS/GO photocatalyst and preparation method thereof

Publications (1)

Publication Number Publication Date
CN116493031A true CN116493031A (en) 2023-07-28

Family

ID=87315675

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310275866.2A Pending CN116493031A (en) 2023-03-21 2023-03-21 Tremella-like Al, N-In 2 S 3 CdS/GO photocatalyst and preparation method thereof

Country Status (1)

Country Link
CN (1) CN116493031A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018058733A (en) * 2016-10-06 2018-04-12 三井化学株式会社 Method for producing metal compound, method for producing photocatalyst, and method for producing photocatalyst complex
CN113634244A (en) * 2021-08-24 2021-11-12 青岛科技大学 High-index crystal face GO @ Cd rich in sulfur vacancy1-xZnxS-shaped polyhedral material and preparation method thereof
CN114669741A (en) * 2022-03-10 2022-06-28 中国科学院生态环境研究中心 Nitrogen-doped carbon-coated aluminum material and preparation method and application thereof
CN115739123A (en) * 2022-11-24 2023-03-07 华东理工大学 CdS/Znln 2 S 4 Preparation method and application of heterojunction photocatalyst

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018058733A (en) * 2016-10-06 2018-04-12 三井化学株式会社 Method for producing metal compound, method for producing photocatalyst, and method for producing photocatalyst complex
CN113634244A (en) * 2021-08-24 2021-11-12 青岛科技大学 High-index crystal face GO @ Cd rich in sulfur vacancy1-xZnxS-shaped polyhedral material and preparation method thereof
CN114669741A (en) * 2022-03-10 2022-06-28 中国科学院生态环境研究中心 Nitrogen-doped carbon-coated aluminum material and preparation method and application thereof
CN115739123A (en) * 2022-11-24 2023-03-07 华东理工大学 CdS/Znln 2 S 4 Preparation method and application of heterojunction photocatalyst

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
MINGHAO ZHANG: "Constructing In2S3/CdS/N-rGO Hybrid Nanosheets via One-Pot Pyrolysis for Boosting and Stabilizing Visible Light-Driven Hydrogen Evolution", 《MOLECULES》, vol. 28, 30 November 2023 (2023-11-30) *
MUHAMMAD NAWAZ: "Preparation of indium-cadmium sulfide nanoparticles with diverse morphologies: Photocatalytic and cytotoxicity study", 《JOURNAL OF MOLECULAR STRUCTURE》, vol. 1253, 30 December 2021 (2021-12-30), pages 1 - 7 *
R. SHEIDA: "Atmospheric pressure non-thermal plasma-liquid interactions for a template-free synthesis of Al-doped CdS nanorods", 《PHOTONICS AND NANOSTRUCTURES-FUNDAMENTALS AND APPLICATIONS》, vol. 37, 17 October 2019 (2019-10-17), XP085904665, DOI: 10.1016/j.photonics.2019.100746 *

Similar Documents

Publication Publication Date Title
Mei et al. A Z-scheme Bi 2 MoO 6/CdSe-diethylenetriamine heterojunction for enhancing photocatalytic hydrogen production activity under visible light
CN109589991B (en) Zinc indium sulfide/copper indium sulfide two-dimensional heterojunction photocatalyst, and preparation method and application thereof
CN110252352B (en) Carbon quantum dot modified bismuth tungstate/ordered macroporous fluorine-doped tin oxide composite photocatalyst and preparation method and application thereof
CN112195483B (en) Method for constructing Z-type heterojunction photo-anode and Z-type heterojunction photo-anode
Zheng et al. A visible-light active pn heterojunction ZnO/Co3O4 composites supported on Ni foam as photoanode for enhanced photoelectrocatalytic removal of methylene blue
CN110624583A (en) Preparation method of composite graphite phase carbon nitride heterojunction photocatalyst
CN110624563A (en) Preparation method of silver ion doped zinc thioindate heterojunction photocatalyst
CN114588888A (en) Photocatalyst and preparation method and application thereof
CN105817217A (en) SrTiO3/graphene composite catalyst as well as preparation method and application thereof
CN110961133B (en) Nonmetal BCN/g-C3N4Van der Waals heterojunction photocatalyst and preparation method and application thereof
Kuspanov et al. Multifunctional strontium titanate perovskite-based composite photocatalysts for energy conversion and other applications
CN115007174A (en) Two-dimensional CdIn 2 S 4 Nanosheet and preparation method and application thereof
CN111203256A (en) SnS2/Au/g-C3N4Preparation method and application of composite photocatalyst
CN114377708A (en) Oxygen vacancy-containing bismuthyl carbonate nanosheet and preparation method and application thereof
CN103272617A (en) CdS/Bi2S3 composite photocatalyst and preparation method thereof
Li et al. Chemical etching and phase transformation of Nickel-Cobalt Prussian blue analogs for improved solar-driven water-splitting applications
CN112371113A (en) Bi2WO6Preparation method and application of-rGO visible light catalyst
WO2023272413A1 (en) Application of tin disulfide nanocatalyst in production of hydrogen by piezoelectric catalytic decomposition of water
CN116493031A (en) Tremella-like Al, N-In 2 S 3 CdS/GO photocatalyst and preparation method thereof
CN113634244B (en) High-index crystal face GO@Cd rich in sulfur vacancies 1-x Zn x S polyhedral material and preparation method thereof
CN113559856B (en) Preparation method of barium titanate/silver iodate heterojunction photocatalyst
CN110876945B (en) ZnIn grown in limited area in carbon nano hollow sphere2S4Photocatalyst and preparation method thereof
Zhang et al. Hierarchical hollow TiO 2/In 2 S 3 heterojunction photocatalyst decorated with spatially separated dual co-catalysts for enhanced photocatalytic H 2 evolution
CN108654673B (en) Novel photocatalytic material and preparation method and application thereof
Salehmin et al. Application of Self-supported Materials for Photo and Photoelectrocatalysis

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination