CN108435210B - Cadmium niobate/cadmium sulfide composite photocatalyst and preparation method thereof - Google Patents

Cadmium niobate/cadmium sulfide composite photocatalyst and preparation method thereof Download PDF

Info

Publication number
CN108435210B
CN108435210B CN201810274932.3A CN201810274932A CN108435210B CN 108435210 B CN108435210 B CN 108435210B CN 201810274932 A CN201810274932 A CN 201810274932A CN 108435210 B CN108435210 B CN 108435210B
Authority
CN
China
Prior art keywords
cadmium
composite photocatalyst
niobate
sulfide composite
preparation
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.)
Expired - Fee Related
Application number
CN201810274932.3A
Other languages
Chinese (zh)
Other versions
CN108435210A (en
Inventor
林华香
张华磊
王绪绪
戴文新
员汝胜
龙金林
张子重
金玉博
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.)
Fuzhou University
Original Assignee
Fuzhou University
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 Fuzhou University filed Critical Fuzhou University
Priority to CN201810274932.3A priority Critical patent/CN108435210B/en
Publication of CN108435210A publication Critical patent/CN108435210A/en
Application granted granted Critical
Publication of CN108435210B publication Critical patent/CN108435210B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

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
    • B01J27/02Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04Sulfides
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a cadmium niobate/cadmium sulfide composite photocatalyst and a preparation method thereof. Firstly, mixing a cadmium source, a niobium source and an organic solvent, drying at 10-100 ℃ under normal pressure, volatilizing the solvent to form powder, then carrying out high-temperature treatment to obtain a precursor of the cadmium niobate/cadmium sulfide composite photocatalyst, and mixing and stirring the precursor in an inorganic salt aqueous solution containing sulfur ions to obtain the cadmium niobate/cadmium sulfide composite photocatalyst. The invention adopts a solvent self-volatilization method to prepare a precursor of the cadmium niobate/cadmium sulfide composite photocatalyst for the first time, and then prepares the composite photocatalyst by an ion exchange method; the obtained composite photocatalyst has a wider light absorption range, and can effectively separate photoproduction electrons from holes, so that the photocatalytic utilization efficiency is improved.

Description

Cadmium niobate/cadmium sulfide composite photocatalyst and preparation method thereof
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a cadmium niobate/cadmium sulfide composite photocatalyst and a preparation method thereof.
Background
Since the second half of the twentieth century, fossil energy has been nearly exhausted with the rapid development of industrialization. Meanwhile, due to the overuse of fossil fuels, environmental pollution reaches unprecedented severe degree. The development of new and efficient clean energy has become a major task faced by the scientific and technical world. The photocatalytic technology can decompose water to produce clean hydrogen energy and convert greenhouse gas CO into CO2Reducing the carbon-containing organic matter again, thereby arousing wide research interest at home and abroad. The development of a novel composite photocatalytic material expands the solar energy utilization rate of the material and improves the quantum conversion efficiency of photocatalytic reaction, which is the core of photocatalytic research and is also the bottleneck problem that future practical application of photocatalytic technology must break through.
Many materials are applied to the research of photocatalysis technology for more than forty years of development of photocatalysis technology, and niobate compounds are in a large numberThe photocatalytic material is unique. The niobate has unique crystal structure and physical and chemical properties, and has the advantages of good thermal stability and high photocatalytic activity when being applied to degradation of organic dyes, photocatalytic hydrogen production and oxygen production and the like. Choi reported KNbO3The loaded CdS can effectively improve the photocatalytic hydrogen production activity under the condition that nickel oxide is used as a cocatalyst, and KNbO3Exhibit excellent carrier and promoting effects.
Cadmium niobate is also a material which is always concerned in niobate, and due to the piezoelectric effect and the photoluminescence effect which are peculiar to cadmium niobate, cadmium niobate is often used as piezoelectric materials, ferroelectric materials, microwave dielectric ceramics and the like instead of the traditional lead-containing heavy metal materials, but the research on the application of photocatalysis is less at present.
Disclosure of Invention
The invention aims to provide a cadmium niobate/cadmium sulfide composite photocatalyst and a preparation method thereof. The composite photocatalyst has a wider light absorption range, and the composite rate of photo-generated electrons and holes is low, so that the photocatalytic utilization efficiency can be effectively improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a cadmium niobate/cadmium sulfide composite photocatalyst is prepared by mixing a niobium source and a cadmium source in an organic solvent, performing solvent self-volatilization and high-temperature roasting to form a cadmium niobate/cadmium sulfide composite photocatalyst precursor, and then preparing the cadmium niobate/cadmium sulfide composite photocatalyst by an ion exchange method; the preparation method specifically comprises the following steps:
1) adding a niobium source and a cadmium source into a 10-100mL bottle according to the molar ratio of metal atoms Nb to Cd being 4: 1-1: 4, adding an organic solvent according to the molar weight of Nb being 1-10000 times, mixing and stirring for 1-6 h, and drying at 10-100 ℃ under normal pressure to obtain a mixture;
2) placing the mixture obtained in the step 1) in a muffle furnace, roasting for 1-24h at 100-600 ℃, obtaining white powder in a bottle, and scraping the powder by using a plastic scraper to obtain a cadmium niobate/cadmium sulfide composite photocatalyst precursor;
3) adding the precursor of the cadmium niobate/cadmium sulfide composite photocatalyst obtained in the step 2) into an inorganic salt aqueous solution with the sulfur ion content of 0.01-2mol/L, mixing and stirring for 1-2 h, sequentially performing vacuum filtration, deionized water washing and ethanol washing, and baking for 2-10h at 40-100 ℃ to obtain the cadmium niobate/cadmium sulfide composite photocatalyst.
Wherein the niobium source is one or more of niobium chloride, niobium oxalate, niobium fluoride and niobium oxide.
The cadmium source is one or more of cadmium chloride, cadmium oxalate, cadmium acetate, cadmium nitrate and cadmium fluoride.
The organic solvent is one or more of methanol, ethanol, formaldehyde, acetaldehyde, acetone and benzene.
The inorganic salt is one or more of sodium sulfide, sodium hydrosulfide, potassium sulfide and ammonium sulfide.
Compared with the prior art, the invention has the remarkable advantages that:
(1) the composite photocatalyst obtained by the invention has a wider light absorption range, and can effectively separate photoproduction electrons from holes, thereby obviously improving the photocatalytic utilization efficiency.
(2) The invention adopts the method of solvent self-volatilization to prepare the composite photocatalyst for the first time, has simple operation, can synthesize the composite photocatalyst by one-time heating, and can effectively save energy consumption.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
Adding niobium oxalate and cadmium fluoride into a 25mL bottle according to the molar ratio of metal atoms Nb to Cd being 4:1, adding ethanol according to 100 times of the molar weight of Nb atoms, mixing and stirring for 1h, and drying at 40 ℃ under normal pressure to obtain a mixture; placing the obtained mixture in a muffle furnace, roasting for 4h at 500 ℃, obtaining white powder in a bottle, and scraping the powder by using a plastic scraper to obtain a precursor of the cadmium niobate/cadmium sulfide composite photocatalyst; adding the obtained precursor of the cadmium niobate/cadmium sulfide composite photocatalyst into a sodium sulfide aqueous solution with the sulfur ion content of 0.1mol/L, mixing and stirring for 2 hours, sequentially performing vacuum filtration, deionized water washing and ethanol washing, and baking at 80 ℃ for 6 hours to obtain the cadmium niobate/cadmium sulfide composite photocatalyst.
Example 2
Adding niobium chloride and cadmium fluoride into a 40mL bottle according to the molar ratio of metal atoms Nb to Cd being 3:1, adding propanol according to 300 times of the molar weight of Nb atoms, mixing and stirring for 1h, and drying at 40 ℃ under normal pressure to obtain a mixture; placing the obtained mixture in a muffle furnace, roasting for 6 hours at 300 ℃, obtaining white powder in a bottle, and scraping the powder by using a plastic scraper to obtain a precursor of the cadmium niobate/cadmium sulfide composite photocatalyst; adding the obtained precursor of the cadmium niobate/cadmium sulfide composite photocatalyst into a potassium sulfide aqueous solution with the sulfur ion content of 0.5mol/L, mixing and stirring for 2 hours, sequentially performing vacuum filtration, deionized water washing and ethanol washing, and baking at 70 ℃ for 5 hours to obtain the cadmium niobate/cadmium sulfide composite photocatalyst.
Example 3
Adding niobium oxalate and cadmium acetate into a 25mL bottle according to the molar ratio of metal atoms Nb to Cd being 1:1, adding methanol according to 500 times of the molar weight of Nb atoms, mixing and stirring for 6h, and drying at 50 ℃ under normal pressure to obtain a mixture; placing the obtained mixture in a muffle furnace, roasting for 4h at 500 ℃, obtaining white powder in a bottle, and scraping the powder by using a plastic scraper to obtain a precursor of the cadmium niobate/cadmium sulfide composite photocatalyst; adding the obtained precursor of the cadmium niobate/cadmium sulfide composite photocatalyst into an ammonium sulfide aqueous solution with the sulfur ion content of 1.5mol/L, mixing and stirring for 1.5h, sequentially performing vacuum filtration, deionized water washing and ethanol washing, and baking at 60 ℃ for 8h to obtain the cadmium niobate/cadmium sulfide composite photocatalyst.
Example 4
Adding niobium chloride and cadmium chloride into a 100mL bottle according to the molar ratio of metal atoms Nb to Cd being 1:2, adding acetone according to 200 times of the molar weight of Nb atoms, mixing and stirring for 5h, and drying at 40 ℃ under normal pressure to obtain a mixture; placing the obtained mixture in a muffle furnace, roasting for 8 hours at 400 ℃, obtaining white powder in a bottle, and scraping the powder by using a plastic scraper to obtain a precursor of the cadmium niobate/cadmium sulfide composite photocatalyst; adding the obtained precursor of the cadmium niobate/cadmium sulfide composite photocatalyst into a sodium hydrosulfide aqueous solution with the sulfur ion content of 2mol/L, mixing and stirring for 1h, sequentially performing vacuum filtration, deionized water washing and ethanol washing, and baking at 60 ℃ for 8h to obtain the cadmium niobate/cadmium sulfide composite photocatalyst.
1. Taking 0.1g of the cadmium niobate/cadmium sulfide composite photocatalyst prepared in the above examples 1 to 4, adding the cadmium niobate/cadmium sulfide composite photocatalyst into a solution containing 0.2mol/L of Na2S and Na2SO3In the photocatalytic reactor of the mixed solution, the photocatalytic hydrogen production activity was tested at a rotation speed of 500r/min using natural light as a light source, and the results are shown in table 1.
TABLE 1 catalytic activity of the cadmium niobate/cadmium sulfide composite photocatalyst prepared in the example of the present invention
Figure DEST_PATH_IMAGE002
2. The hydrogen production activity of the cadmium niobate/cadmium sulfide composite photocatalyst prepared in example 3 was compared with that of the existing cadmium sulfide, niobium titanate/cadmium sulfide (the preparation method is described in connection with the preparation of a xiong "CdS pillared titanium niobate mesoporous composite material and the hydrogen production activity by photolysis of water"), niobium nitride/cadmium sulfide (the preparation method is described in connection with CN 105854924a, "a preparation method of a niobium nitride/cadmium sulfide composite nanoparticle photocatalyst"), and niobium pentoxide/cadmium sulfide (the preparation method is described in connection with the preparation of a yuezen "niobium-based composite material and the research on the photocatalytic hydrogen production performance thereof) under the same conditions, and the results are shown in table 2.
TABLE 2 comparison of hydrogen production activities of different catalytic materials
Figure DEST_PATH_IMAGE004
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 (5)

1. A preparation method of a cadmium niobate/cadmium sulfide composite photocatalyst is characterized by comprising the following steps: the method comprises the following steps:
1) adding a niobium source and a cadmium source into a bottle according to the molar ratio of metal atoms Nb to Cd being 4: 1-1: 4, adding an organic solvent according to 1-10000 times of the molar weight of Nb atoms, mixing and stirring for 1-6 h, and drying at 10-100 ℃ under normal pressure to obtain a mixture;
2) placing the mixture obtained in the step 1) in a muffle furnace, and roasting for 1-24h at 100-600 ℃ to obtain a precursor of the cadmium niobate/cadmium sulfide composite photocatalyst;
3) adding the cadmium niobate/cadmium sulfide composite photocatalyst precursor obtained in the step 2) into an inorganic salt aqueous solution with the sulfur ion content of 0.01-2mol/L, mixing and stirring for 1-2 h, sequentially performing vacuum filtration, deionized water washing and ethanol washing, and baking at 40-100 ℃ for 2-10h to obtain the cadmium niobate/cadmium sulfide composite photocatalyst;
the organic solvent is one or more of methanol, ethanol, formaldehyde, acetaldehyde, acetone and benzene.
2. The preparation method of the cadmium niobate/cadmium sulfide composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: the niobium source is one or more of niobium chloride, niobium oxalate, niobium fluoride and niobium oxide.
3. The preparation method of the cadmium niobate/cadmium sulfide composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: the cadmium source is one or more of cadmium chloride, cadmium oxalate, cadmium acetate, cadmium nitrate and cadmium fluoride.
4. The preparation method of the cadmium niobate/cadmium sulfide composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: the inorganic salt is one or more of sodium sulfide, sodium hydrosulfide, potassium sulfide and ammonium sulfide.
5. The cadmium niobate/cadmium sulfide composite photocatalyst prepared by the method of claim 1.
CN201810274932.3A 2018-03-30 2018-03-30 Cadmium niobate/cadmium sulfide composite photocatalyst and preparation method thereof Expired - Fee Related CN108435210B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810274932.3A CN108435210B (en) 2018-03-30 2018-03-30 Cadmium niobate/cadmium sulfide composite photocatalyst and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810274932.3A CN108435210B (en) 2018-03-30 2018-03-30 Cadmium niobate/cadmium sulfide composite photocatalyst and preparation method thereof

Publications (2)

Publication Number Publication Date
CN108435210A CN108435210A (en) 2018-08-24
CN108435210B true CN108435210B (en) 2020-10-09

Family

ID=63198286

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810274932.3A Expired - Fee Related CN108435210B (en) 2018-03-30 2018-03-30 Cadmium niobate/cadmium sulfide composite photocatalyst and preparation method thereof

Country Status (1)

Country Link
CN (1) CN108435210B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115304101B (en) * 2022-08-22 2023-10-27 福州大学 Cadmium niobate nano material and preparation method and application thereof
CN116078439A (en) * 2022-09-08 2023-05-09 上海理工大学 Two-dimensional material modified zirconium-based catalyst and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105709793A (en) * 2016-01-26 2016-06-29 苏州大学 Cadmium sulfide nanoparticle modified niobium pentoxide nanorod/nitrogen doped graphene composite photocatalyst and preparation method and application thereof
CN106964379A (en) * 2017-03-23 2017-07-21 福州大学 Contain ZnI with photocatalysis antibacterial function2The preparation method of I/ZnO composites
CN107381635A (en) * 2017-08-07 2017-11-24 武汉工程大学 A kind of Bi2Ti2O7Ceramic powder and preparation method thereof
CN107376943A (en) * 2017-07-20 2017-11-24 江苏大学 A kind of preparation method and purposes of calcium niobate potassium/cadmium sulfide composite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105709793A (en) * 2016-01-26 2016-06-29 苏州大学 Cadmium sulfide nanoparticle modified niobium pentoxide nanorod/nitrogen doped graphene composite photocatalyst and preparation method and application thereof
CN106964379A (en) * 2017-03-23 2017-07-21 福州大学 Contain ZnI with photocatalysis antibacterial function2The preparation method of I/ZnO composites
CN107376943A (en) * 2017-07-20 2017-11-24 江苏大学 A kind of preparation method and purposes of calcium niobate potassium/cadmium sulfide composite material
CN107381635A (en) * 2017-08-07 2017-11-24 武汉工程大学 A kind of Bi2Ti2O7Ceramic powder and preparation method thereof

Also Published As

Publication number Publication date
CN108435210A (en) 2018-08-24

Similar Documents

Publication Publication Date Title
CN108714431B (en) Nano-cellulose reinforced composite photocatalyst and preparation method and application thereof
CN105817253B (en) The preparation method of graphite phase carbon nitride nanometer sheet/Nano tube array of titanium dioxide catalysis material
CN103638923B (en) A kind of rare earth element nd doping Bi 2wO 6composite photo-catalyst and its preparation method and application
CN111705419B (en) Metal-loaded carbon nitride-doped graphene-based flexible non-woven fabric and preparation method and application thereof
CN102674451A (en) Preparation method of {001} face exposed titanium dioxide nanocrystals
CN103100398A (en) Preparation method of natural zeolite loaded one-dimensional TiO2 nanowire with high catalytic activity
CN106540673A (en) A kind of three-dimensional TiO2The synthetic method of/ZnO heterojunction array
CN112958116B (en) Bi2O2.33-CdS composite photocatalyst and preparation process thereof
CN109759119B (en) Molybdenum carbide modified tubular carbon nitride photocatalytic material and preparation method and application thereof
CN108435210B (en) Cadmium niobate/cadmium sulfide composite photocatalyst and preparation method thereof
CN105039938A (en) Method for preparing photoelectrode of alpha-iron oxide film by single-source precursor
CN113086955A (en) Preparation method of carbon-deficient carbon nitride material for photocatalytic nitrogen fixation
CN107352519B (en) A kind of C3N4The preparation method of nano wire
CN102553562B (en) Multiple modified composite photocatalyst and preparation method thereof
CN102173450A (en) Preparation method of titanium dioxide film
CN103611527B (en) A kind of visible light-responded Ce doping Bi 2wO 6crystallite and its preparation method and application
CN104971753A (en) Bi2O2CO3-BiPO4 composite photocatalyst and preparation method thereof
CN111933962B (en) N, S co-doped metal-free CNS oxygen reduction catalyst and preparation method thereof
CN104028309A (en) Composite type visible-light-induced photocatalyst and preparation method thereof
CN113304769B (en) A series of bimetallic silicates/g-C 3 N 4 Preparation and application of composite photocatalyst
CN108465464B (en) Preparation method and application of barium strontium titanate/bismuth vanadate
CN110624532B (en) TiO 22-BiVO4-graphene ternary composite photocatalytic material and preparation method thereof
CN112657518A (en) Carbon dioxide reduction composite photocatalytic material and preparation method thereof
CN110711585B (en) Tree crown-shaped anoxic tin oxide nanosheet array structure and preparation method thereof
CN109913892B (en) Method for photoelectrocatalytic oxidation of xylose by indium sulfide/nickel iron hydrotalcite composite membrane

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
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20201009

CF01 Termination of patent right due to non-payment of annual fee