CN114618527A - Niobate composite nanomaterial modified by Au nanoparticles and CdS quantum dots and application thereof - Google Patents
Niobate composite nanomaterial modified by Au nanoparticles and CdS quantum dots and application thereof Download PDFInfo
- Publication number
- CN114618527A CN114618527A CN202210288080.XA CN202210288080A CN114618527A CN 114618527 A CN114618527 A CN 114618527A CN 202210288080 A CN202210288080 A CN 202210288080A CN 114618527 A CN114618527 A CN 114618527A
- Authority
- CN
- China
- Prior art keywords
- niobate
- cds
- hnb
- mixed solution
- quantum dots
- 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.)
- Granted
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 45
- 239000002096 quantum dot Substances 0.000 title claims abstract description 42
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims description 37
- 239000002135 nanosheet Substances 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000011941 photocatalyst Substances 0.000 claims description 26
- 239000000725 suspension Substances 0.000 claims description 26
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 24
- 229910001868 water Inorganic materials 0.000 claims description 23
- 230000001699 photocatalysis Effects 0.000 claims description 20
- 239000002244 precipitate Substances 0.000 claims description 20
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 17
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 17
- OGMADIBCHLQMIP-UHFFFAOYSA-N 2-aminoethanethiol;hydron;chloride Chemical compound Cl.NCCS OGMADIBCHLQMIP-UHFFFAOYSA-N 0.000 claims description 14
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 13
- 229940097265 cysteamine hydrochloride Drugs 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- ZTILUDNICMILKJ-UHFFFAOYSA-N niobium(v) ethoxide Chemical compound CCO[Nb](OCC)(OCC)(OCC)OCC ZTILUDNICMILKJ-UHFFFAOYSA-N 0.000 claims description 11
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 11
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 9
- 229940043267 rhodamine b Drugs 0.000 claims description 9
- 239000012265 solid product Substances 0.000 claims description 9
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 8
- 229940012189 methyl orange Drugs 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000084 colloidal system Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 230000000593 degrading effect Effects 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 4
- JKYKXTRKURYNGW-UHFFFAOYSA-N 3,4-dihydroxy-9,10-dioxo-9,10-dihydroanthracene-2-sulfonic acid Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C(O)=C(O)C(S(O)(=O)=O)=C2 JKYKXTRKURYNGW-UHFFFAOYSA-N 0.000 claims description 2
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 claims description 2
- 239000002055 nanoplate Substances 0.000 claims description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 14
- 230000015556 catabolic process Effects 0.000 abstract description 13
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000013032 photocatalytic reaction Methods 0.000 abstract description 5
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 239000010931 gold Substances 0.000 description 70
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 22
- 239000000243 solution Substances 0.000 description 16
- 239000000975 dye Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000002114 nanocomposite Substances 0.000 description 8
- 239000012153 distilled water Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- 238000000862 absorption spectrum Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000010955 niobium Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000010842 industrial wastewater Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- BQSPOPBPQURHDF-JJYYJPOSSA-N (4s,5s)-2-amino-5-[(1r)-2-amino-1-hydroxyethyl]-4,5-dihydro-1h-imidazole-4-carboxylic acid Chemical compound NC[C@@H](O)[C@H]1NC(N)=N[C@@H]1C(O)=O BQSPOPBPQURHDF-JJYYJPOSSA-N 0.000 description 2
- 101100220616 Caenorhabditis elegans chk-2 gene Proteins 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002060 nanoflake Substances 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000001782 photodegradation Methods 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 238000000527 sonication Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- LEVWYRKDKASIDU-IMJSIDKUSA-N L-cystine Chemical compound [O-]C(=O)[C@@H]([NH3+])CSSC[C@H]([NH3+])C([O-])=O LEVWYRKDKASIDU-IMJSIDKUSA-N 0.000 description 1
- 239000004158 L-cystine Substances 0.000 description 1
- 235000019393 L-cystine Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229960003067 cystine Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000013460 polyoxometalate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910009112 xH2O Inorganic materials 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/20—Sulfiding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to the technical field of nano materials, and particularly relates to a niobate composite nano material modified by Au nano particles and CdS quantum dots and application thereof. The invention loads Au nano-particles and CdS quantum dots to niobate nano-particlesPreparing the niobate composite nano material HNb modified by Au nano particles and CdS quantum dots on a chip3O8Au/CdS. The composite nano material HNb loaded with nano particles (Au) and quantum dots (CdS)3O8the/Au/CdS composite material has a high specific surface area, so that more active sites can be provided for adsorbing pollutants, and the photocatalytic reaction can be facilitated. The operation method is simple, the preparation conditions are easy to control, the preparation process method has the characteristic of no pollution, and the prepared niobate composite nanomaterial modified by the Au nanoparticle and the CdS quantum dot has the advantages of good catalytic effect, high degradation rate and high application value.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a niobate composite nano material modified by Au nano particles and CdS quantum dots and application thereof.
Background
The niobate has potential application value in the aspects of photocatalysis, microbiology, nuclear waste treatment, catalytic degradation of organic pollutants and the like due to the unique characteristics of high charge, high specific surface area, high alkalinity and the like. In recent years, it is a trend of research to obtain new materials or hybrid materials with enhanced performance by compounding different materials and utilizing the synergistic effect of each material component.
The prior art has thus far disclosed a variety of nanocomposites with different morphologies and properties. For example, Zhang Guanjin et al enhanced the photocatalytic activity of nanocomposites by Self-assembly of polyoxometalate-coated Au nanoparticles and CdS quantum dots in 2013 (see document Xing X, Liu R, Yu X, et al. Self-assembly of CdS quantum dots with polyoxometalate-encapsulated gold nanoparticles J]Journal of Materials Chemistry A, 2013, 1(4): 1488-1494). Subsequently, Cd was studied by the Yan subject group0.65Zn0.35S nanoparticles, and mixing Nb6And NiS as a cocatalyst to form nanocomposites (see Ma L, Li F, Sun Z, et al. synthetic effect of polyoxinobate and NiS as catalysts for enhanced photocatalytic H2 evolution on Cd0.65Zn0.35S [J]RSC Advances, 2014, 4(41): 21369-. In 2017, the Wansheng group successfully synthesized the poly niobate-CdS nanocomposite under mild hydrothermal conditions by using L-cystine biomolecules as a sulfur source and a complexing agent (see Liu M, Chen H, ZHao H, et al, biomolecular-mediated hydrothermatic synthesis of polyoxoacetate-CdS nanohybrids with enhanced photocatalytic reaction for hydrogen production and RhB degradation [ J M, Chen H, ZHao H, et al]. Dalton Transactions, 2017, 46(29): 9407-9414）。
In the above studies, CdS as a semiconductor material for preparing a photocatalyst is not used, and CdS as an important semiconductor material has been favored by researchers in the field of photocatalysis, but the research on preparing a photocatalyst by modifying a nanomaterial with niobate is relatively less.
The photocatalyst is used for catalyzing and decomposing organic substances harmful to human bodies and the environment, and has important effects on saving resources and avoiding environmental pollution. Therefore, the research and development of the semiconductor composite nano material with better photocatalytic performance have important significance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a composite nano material HNb loaded with nano particles (Au) and quantum dots (CdS)3O8the/Au/CdS composite material has a high specific surface area, so that more active sites can be provided for adsorbing pollutants, and the photocatalytic reaction can be facilitated.
The invention also provides a preparation method of the composite nano material loaded with the nano particles and the quantum dots.
The invention further provides application of the composite nano material loaded with the nano particles and the quantum dots in the aspect of photocatalytic hydrogen production and application in the aspect of artificial dye degradation.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a preparation method of a niobate composite nano material modified by CdS quantum dots comprises the following steps:
a. the preparation method of the niobate nanosheet comprises the following steps of taking an amino surfactant (niobium ethoxide in the application) as a raw material, and synthesizing the niobate nanosheet in an ammonia water solution by adopting a hydrothermal method, wherein the preparation method comprises the following specific steps: mixing niobium ethoxide and Triethanolamine (TEOA) to obtain a mixed solution I, adjusting the pH value of the mixed solution I to 12-13, reacting at 120-180 ℃ for 12-24 hours to obtain a colloidal suspension, removing a precipitate part, collecting a light yellow supernatant colloid, centrifuging to obtain a solid product, washing and drying to obtain niobate (HNb)3O8) Nano-sheet；
b. HNb3O8Preparation of a/CdS composite material: b, mixing the niobate nanosheets and CdCl in the step a2、Na2S and cysteamine hydrochloride are dissolved in water to obtain a mixed solution II, the mixed solution II reacts for 5 to 10 hours at the temperature of 40 to 50 ℃ to obtain a yellow green suspension, the yellow green suspension is cooled to room temperature, precipitate is separated, washed and dried to obtain yellow powder HNb3O8/CdS。
Specifically, the mass ratio of niobium ethoxide to triethanolamine in the step a is 1: (2-10).
Specifically, the step a comprises the following steps: dissolving 0.663 g niobium ethoxide in 1.32-6.63 g triethanolamine, adding NH3·H2O to adjust pH to 12.8, then placing the mixed solution I in a high pressure reactor to age at 160 ℃ for 24 hours, cooling to room temperature, then centrifuging the product at 6000 rpm for 10 minutes to obtain a colloidal suspension containing a small amount of white precipitate, removing the precipitate portion, collecting a pale yellow supernatant colloid, centrifuging to obtain a solid product, washing with distilled water, and vacuum-drying the product at 80 ℃ for 12 hours.
In particular, ammonia (NH) used for adjusting pH in step a3) The content is 25-28%, the purpose is to make the niobate nano-sheet precipitate out better and faster under the alkaline environment, and preferably, ammonium hydroxide can be used to replace ammonia water.
Specifically, CdCl in step b2With Na2The molar ratio of S is 1: (1-2).
Specifically, the molar ratio of the niobate nanosheets to the CdS in the step b is 5 (1-5).
Specifically, the step b comprises the following steps: dispersing 0.094 g of the niobate nanosheets obtained in the step a into 30-50 mL of distilled water through ultrasonic treatment, and then adding 0.046-0.3 g of CdCl20.048-0.23 g of Na2S and 0.059-0.284 g of cysteamine hydrochloride to obtain a mixed solution II, and reacting the mixed solution II at 40 ℃ for 5 hours, and then reacting at 60 ℃ for 5 hours to obtain uniform yellow-green suspension; cooling to room temperature, separating precipitate, washing precipitate with isopropanol and water, and cooling at 40 deg.CVacuum drying for 24 h and collecting to obtain yellow powder HNb3O8/CdS。
Further, the invention also provides a preparation method of the niobate composite nanomaterial modified by the Au nanoparticles and the CdS quantum dots, which comprises the following steps:
(1) preparing niobate nano sheets: mixing niobium ethoxide with Triethanolamine (TEOA) to obtain a mixed solution I, adjusting the pH of the mixed solution I to be 12-13, reacting at 120-180 ℃ for 12-24 hours to obtain a colloidal suspension, removing a precipitate part, collecting a light yellow supernatant colloid, centrifuging to obtain a solid product, washing and drying to obtain the niobate (HNb)3O8) Nanosheets;
（2）HNb3O8preparing a/Au/CdS composite material: dissolving the niobate flakes and chloroauric acid in the step (1) in water to obtain a mixed solution III, stirring and irradiating the mixed solution III with a xenon lamp for 30-60min to obtain a purple gray suspension, centrifuging, collecting a product, washing with water, and drying to obtain Au-modified niobate flakes;
then adding the Au modified niobate nano-sheet and CdCl2、Na2S and cysteamine hydrochloride are dissolved in water to obtain a mixed solution IV, the mixed solution IV reacts for 5 to 10 hours at the temperature of 40 to 50 ℃ to obtain a yellow-green suspension, the yellow-green suspension is cooled to room temperature, precipitate is separated, washed and dried to obtain yellow-green powder HNb3O8/Au/CdS。
Further, in the step (1), the mass ratio of niobium ethoxide to triethanolamine is 1: (2-10).
Further, the specific steps in the step (2) are as follows: dispersing niobate sheets in distilled water through ultrasonic treatment, then adding chloroauric acid to obtain a mixed solution III, irradiating the mixed solution III for 30 minutes by using a xenon lamp under the condition of vigorous stirring to obtain purple gray turbid liquid, centrifuging, collecting a product, washing with water, and drying to obtain Au modified niobate nano sheets.
Further, the mass ratio of the Au-modified niobate nano-sheets to the cysteamine hydrochloride in the step (2) is (0.3-1.6): 1.
Further, the method can be used for preparing a novel materialThe specific steps in the step (2) are as follows: dissolving 0.094 g of Au modified niobate nano-sheet in 30-50 mL of water, and adding 0.046-0.3 g of CdCl20.048-0.23 g of Na2S and 0.059-0.284 g of cysteamine hydrochloride to obtain a mixed solution IV, reacting the mixed solution IV at 40 ℃ for 5 h, continuing to react at 60 ℃ for 5 h, stirring vigorously during the reaction process to obtain a yellow-green suspension with uniform texture, cooling to room temperature, separating precipitate, washing the precipitate with isopropanol and water, vacuum drying at 60 ℃ for 24 h, and collecting to obtain yellow-green powder HNb3O8/Au/CdS。
In the method, the niobate composite nanomaterial HNb modified by the Au nanoparticles and the CdS quantum dots is prepared by loading the Au nanoparticles and the CdS quantum dots on the niobate nanoparticles3O8/Au/CdS。
Further, the invention also provides a niobate composite nano material HNb modified by the CdS quantum dots3O8/CdS or niobate composite nano material HNb modified by Au nano particles and CdS quantum dots3O8The application of the/Au/CdS serving as a photocatalyst in photocatalytic hydrogen production.
Specifically, when the method is applied, the steps are as follows: a 300W xenon lamp is used as a light source to carry out modification on the Au nano particles and the CdS quantum dots to obtain the niobate composite nano material HNb3O8And carrying out photocatalytic hydrogen production by Au/CdS, and detecting the content of the produced hydrogen after illumination.
Further, the invention also provides a niobate composite nano material HNb modified by the CdS quantum dots3O8/CdS, or niobate composite nano material HNb modified by Au nano particles and CdS quantum dots3O8Application of/Au/CdS in degrading artificial dye.
Specifically, the artificial dye can be rhodamine B, methylene blue, methyl orange, alizarin red S or Congo red.
Specifically, when the method is applied, the steps are as follows: 3-10 mg of composite nano material HNb3O8Adding Au/CdS into 10-20 mL of concentrated solutionCarrying out ultrasonic treatment for 30-60min in a solution of the artificial dye with the degree of 10-20 mg/L, then placing the solution in white light for reaction, and detecting the degradation rate of the artificial dye.
Compared with the prior art, the invention has the advantages that:
according to the invention, the niobate nanosheets with good properties are synthesized by using the niobate nanosheets as precursors through a water solution synthesis method, and the photocatalytic performance and photodegradation performance of the nano composite material prepared by doping the niobate with the Au-loaded nanoparticles and the CdS quantum dots are explored. The invention not only enriches the diversity of the sheet structure, but also provides a potential method for the functionalization of the nano material.
The operation method is simple, the preparation conditions are easy to control, the preparation process method has the characteristic of no pollution, and the prepared niobate composite nanomaterial modified by the Au nanoparticles and the CdS quantum dots has the advantages of good catalytic effect, high degradation rate and high application value.
Drawings
FIG. 1 shows HNb prepared in example 13O8Scanning electron microscopy of nanoplates and HNb prepared in example 13O8A transmission electron microscope image of/Au/CdS-3, wherein, FIG. 1a is a scanning electron microscope image, and FIGS. 1b-f are transmission electron microscope images;
FIG. 2 is an X-ray powder diffraction pattern of the composite nanomaterials prepared in examples 1-4;
FIG. 3 is HNb of composite nano-material prepared in example 43O8An X-ray photoelectron spectrum of/Au/CdS-3, wherein FIG. 3a is HNb3O8XPS test chart of/Au/CdS-3, FIG. 3b is Nb element, FIG. 3c is Au element, and FIG. 3d is Cd element;
FIG. 4 is a graph of photocatalytic hydrogen production with water as a function of time for composite nanomaterials prepared in examples 1 to 6;
FIG. 5 is a graph showing the degradation effect of the composite nanomaterial prepared in examples 1, 2 and 4 and photocatalysis on Methylene Blue (MB);
FIG. 6 shows the HNb of the composite nanomaterial prepared in example 43O8Au/CdS-3 in process of photodegrading Methylene Blue (MB)Ultraviolet absorption spectrum chart of test in (1);
FIG. 7 shows the HNb of the composite nanomaterial prepared in example 43O8UV absorption spectrum chart of Au/CdS-3 tested in the process of photodegradation of rhodamine B (RhB);
FIG. 8 shows the HNb of the composite nanomaterial prepared in example 43O8UV absorption spectrum of Au/CdS-3 tested in the process of photodegrading Methyl Orange (MO).
Detailed Description
The following examples will further illustrate the invention in conjunction with the accompanying drawings. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a process are given, but the scope of the present invention is not limited to the following embodiments.
Wherein the photocatalytic system: CEL-PAEM-D8, beijing; model of photoreactor: WP-TEC-1020 SL; gas chromatograph: TCD detection, GC-7900.
Example 1
HNb3O8Preparation of the nanosheet:
0.663 g of niobium (V) ethoxide (molecular formula is Nb (OEt)5) Mixing with 1.133 mL Triethanolamine (TEOA) to obtain a mixed solution I; by NH3·H2O, adjusting the pH value of the mixed solution I to keep the pH value of the mixed solution I at 12.8;
then transferring the mixed solution I into a high-pressure reaction kettle, placing the high-pressure reaction kettle in an oven for aging at 160 ℃ for 24 hours, centrifuging the obtained product at 6000 rpm for 10 minutes to obtain colloidal suspension containing a small amount of white precipitate, removing the precipitate, collecting light yellow supernatant colloid, centrifuging to obtain a solid product, washing the solid product with distilled water for three times, and vacuum-drying the obtained product at 80 ℃ for 12 hours to obtain the niobate (HNb)3O8) And (4) nano flakes.
Example 2
Preparing CdS quantum dots:
0.114 g of cadmium chloride (CdCl)2·2.5H2O), 0.15 g of sodium sulfide (Na)2S·9H2O) and 0.142 g of cysteamine hydrochloride (C: (A)C2H8ClNS, 2-aminoethanethiol hydrochloride) is dissolved in 30 mL deionized water, then the mixture reacts for 5 h at the temperature of 40 ℃, then the mixture continues to react for 5 h at the temperature of 60 ℃, the mixture is stirred vigorously during the reaction process, and yellow colloidal suspension with uniform texture is obtained after the reaction; after the suspension was cooled to room temperature, 15 mL of isopropanol was added to make the solution cloudy, the yellow precipitate was centrifuged, washed with a mixture of water and isopropanol (total volume 30 mL) and centrifuged again, wherein the volume ratio of water to isopropanol was 1:1, and this operation was repeated 3 times; and then carrying out vacuum drying for 24 h at the temperature of 40 ℃ and collecting to obtain a CdS quantum dot product.
Example 3
Preparing a niobate nanosheet composite photocatalyst modified by CdS quantum dots:
0.094 g of the niobate (HNb) of example 1 was added3O8) The nanoflakes were dispersed in 30 mL of distilled water by sonication, followed by the addition of 0.1384 g of cadmium chloride (CdCl)2·2.5H2O), 0.18 g of sodium sulfide (Na)2S·9H2O) and 0.17 g of cysteamine hydrochloride (C)2H8ClNS) to obtain a mixed solution II;
reacting the mixed solution II at 40 ℃ for 5 hours, then continuously reacting at 60 ℃ for 5 hours, and continuously and violently stirring in the reaction process to obtain a light yellow colloid suspension liquid with uniform texture; after the suspension was cooled to room temperature, 15 mL of isopropanol was added to make the solution cloudy, the yellow precipitate was centrifuged, washed with a mixture of water and isopropanol (total volume 30 mL) and centrifuged again, wherein the volume ratio of water to isopropanol was 1:1, and this operation was repeated 3 times; then vacuum drying is carried out for 24 h at the temperature of 40 ℃ and collection is carried out, so as to obtain the CdS quantum dot modified niobate nanosheet composite photocatalyst HNb3O8/CdS。
Example 4
Preparing a niobate nanosheet composite photocatalyst modified by Au nanoparticles and CdS quantum dots:
(1) 0.2 g of the niobate (HNb) of example 1 was added3O8) Nano-flakesDispersed in 30 mL of distilled water by sonication, then 0.06 g of chloroauric acid (HAuCl) was added4·xH2O, the mass percent of gold is 47.8-50 percent), obtaining a mixed solution III, irradiating the mixed solution III for 30 minutes by using a 300W xenon lamp under the condition of vigorous stirring to obtain purple gray suspension, centrifugally separating the suspension, collecting a product, washing with water, and drying to obtain a niobate sheet modified by Au nano particles;
(2) dispersing 0.094 g of the niobate sheet modified by the Au nanoparticles in the step (4) in 30 mL of distilled water through ultrasonic treatment, and then adding 0.138 g of cadmium chloride (CdCl)2·2.5H2O), 0.18 g of sodium sulfide (Na)2S·9H2O) and 0.17 g cysteamine hydrochloride (C)2H8ClNS) to obtain a mixed solution IV;
(3) reacting the mixed solution IV at the temperature of 40 ℃ for 5 hours, then continuously reacting at the temperature of 60 ℃ for 5 hours, and continuously and violently stirring in the reaction process to obtain a yellow-green suspension with uniform texture after reaction; after the suspension was cooled to room temperature, 15 mL of isopropanol was added to make the solution cloudy, the yellow precipitate was centrifuged, washed with a mixture of water and isopropanol (total volume 30 mL) and centrifuged, wherein the volume ratio of water to isopropanol was 1:1, and this operation was repeated 3 times; then vacuum drying is carried out for 24 h at the temperature of 60 ℃ and collection is carried out, so as to obtain the niobate nanosheet composite photocatalyst HNb modified by Au nanoparticles and CdS quantum dots3O8/Au/CdS-3；
HNb in this example3O8The molar ratio of the Au nano particles to the CdS quantum dots is 5:1: 3.
Characterization of the products obtained in examples 1 to 4
Scanning electron microscope and transmission electron microscope are shown in FIG. 1, and FIG. 1a and FIG. 1b show HNb prepared in example 13O8The prepared HNb can be seen from the figure of a scanning electron microscope3O8The nano sheets have good appearance and are arranged orderly.
FIGS. 1c-f are HNb prepared in example 43O8The transmission electron microscope picture of/Au/CdS-3 shows that Au nanoparticles and CdS quantum dots are successfulLoaded on the niobate nano-chip; HNb3O8The lattice spacing of the nanosheets is 0.21 nm, corresponding to the (360) crystal face thereof, the lattice spacing of the Au nanoparticles is 0.24 nm, corresponding to the (111) crystal face thereof, and the lattice spacing of the CdS quantum dots is 0.34 nm, corresponding to the (001) crystal face thereof.
HNb in example 43O8The X-ray powder diffraction of/Au/CdS-3 is shown in FIG. 2, and it can be seen from FIG. 2 that a diffraction peak with stronger intensity appears at 27.7 degrees, corresponding to HNb3O8The (121) crystal plane of (2). The two diffraction peaks detected at 38.3 ° and 44.5 ° correspond to (111) and (200) of Au, respectively. The characteristic peak at 26.6 ° is referred to as the (001) crystal plane of CdS.
HNb in example 43O8The X-ray photoelectron spectrum of Au/CdS-3 is shown in FIG. 3, from which the chemical composition and binding energy of the atoms can be further determined, and Nb 3d peaks corresponding to niobate-containing Nb at 207.1 and 209.8 eV are observed5+(ii) a The peaks at 84.4 and 88.1 eV can be assigned to the binding energy of the 4f orbital of Au nanoparticles. The peaks of Cd 3d at 405.0 and 411.7 eV can be assigned to Cd of CdS particles2+。
Example 5
This example is different from example 4 in that cadmium chloride (CdCl) is used in the step (2)2·2.5H2O) 0.046 g, sodium sulfide (Na)2S·9H2O) mass 0.048 g and cysteamine hydrochloride (C)2H8ClNS) was 0.059 g. The prepared product is a niobate nanosheet composite photocatalyst HNb modified by Au nanoparticles and CdS quantum dots3O8/Au/CdS-1。
HNb in this example3O8The molar ratio of the Au nano particles to the CdS quantum dots is 5:1: 1.
Example 6
This example is different from example 4 in that cadmium chloride (CdCl) is used in step (2)2·2.5H2O) mass was 0.23 g, and sodium sulfide (Na)2S·9H2O) mass 0.30 g and cysteamine hydrochloride (C)2H8ClNS) had a mass of 0.284 g. The prepared product is a niobate nanosheet composite photocatalyst HNb modified by Au nanoparticles and CdS quantum dots3O8/Au/CdS-5。
HNb in this example3O8The molar ratio of the Au nano particles to the CdS quantum dots is 5:1: 5.
Photocatalytic water hydrogen production experiment
The samples prepared in examples 1, 2 and 3 and the nanocomposite samples prepared in examples 4 to 6 were respectively charged into a photoreactor in an amount of 0.05 g. An experiment for photocatalytic hydrogen production was carried out using a 300W xenon lamp as a light source (see Ma D, Shi J-W, Sun D, et al. Au nanoparticles and CdS rectangle dot code of In2O3 nanosheets for improved H2 evolution resulting from efficient light harvesting and charge transfer [J]. ACS Sustainable Chemistry &Engineering, 2018, 7(1): 547-57), samples were taken every 1H and tested for hydrogen production, and H was observed2The resulting amount was varied, and the results are shown in FIG. 4.
FIG. 4 shows the variation of 6 materials of examples 1-6 as photocatalyst with time, and FIG. 4 shows that the composite material HNb prepared in example 33O8The photocatalyst activity of Au/CdS-3 reaches the highest value at 5 h, about 29.24 mmol-g-1And example 3 the composite HNb3O8The photocatalyst activity of/Au/CdS-3 is the highest among the 6 materials. At the same time, it can be seen that pure HNb3O8Is relatively low. In the composite nano material, the activity of the photocatalyst is obviously improved along with the gradual increase of the amount of CdS, but the photocatalytic activity of the composite material is not increased or decreased when the amount of CdS exceeds a certain amount.
Wherein, the composite nanomaterial HNb prepared in example 43O8The performance of the/Au/CdS-3 photocatalyst is optimal; example 6 composite nanomaterial HNb3O8The photocatalytic activity of Au/CdS-5 is lower than that of HNb of the composite nano material prepared in example 23O8Au/CdS-1. The result shows that the visible light catalytic activity of the niobate nanosheet can be improved by a proper amount of CdS quantum dots, and the Au nanoparticles play a key role in photocatalytic reaction.
Experiment for photocatalytic degradation of methylene blue
5 mg of the materials prepared in examples 1 and 2 and the nanocomposite material prepared in example 4 were uniformly dispersed as a photocatalyst in 10 mL of methylene blue solution (10 mg/L) respectively to perform photocatalytic degradation reaction, and before the photocatalytic reaction, the solution was subjected to ultrasonic treatment in the dark for 60min to achieve an adsorption-desorption equilibrium state of the photocatalyst and the dye solution. Subsequently, the solution was placed in a photochemical reactor with white light (light source color temperature of 6000-. Samples were taken every 1H and subjected to UV test analysis (see the test methods FENTIE TADESSE S, Kuo D-H, LAKEW KEBEDE W, et al. Visible light drive Nd2O3/Mo(S,O)3-x·0.34H2O heterojunction for enhanced photocatalytic degradation of organic pollutants [J]. Applied Surface Science, 2021, 569: 151091）。
FIG. 5 is a diagram using HNb3O8、CdS、HNb3O8A concentration change diagram of a solution after the/Au/CdS-3 is used for carrying out photocatalytic degradation on organic Methylene Blue (MB), and only using light irradiation catalysis (Photolysis) to degrade the organic methylene blue without adding a catalyst. As can be seen from the figure, the concentration of methylene blue solution becomes smaller after 4 h of light irradiation, indicating photocatalysis (Photolysis), HNb3O8CdS and HNb3O8Four catalytic conditions of/Au/CdS-3 have certain degradation effect on degrading MB, but HNb is used3O8The degradation rate and efficiency of/Au/CdS-3 to MB are highest. This indicates HNb3O8the/Au/CdS-3 has better degradation effect on MB as a photocatalyst, namely the prepared nano material HNb3O8the/Au/CdS-3 can be used as a photocatalyst and has good application prospect in industrial wastewater treatment.
FIG. 6 is a nanocomposite of example 4Material HNb3O8the/Au/CdS-3 is used as an ultraviolet absorption spectrogram tested in the degradation process of the photocatalyst, and the curves are test results of dark treatment for 1 hour to illumination for 4 hours from top to bottom. As can be seen from FIG. 6, the absorbance of the solution at 4 hours was substantially zero, indicating that the composite nanomaterial HNb produced in example 4 was3O8the/Au/CdS-3 photocatalyst has high activity, and the composite nano material HNb prepared in the example 4 is also shown3O8The Au/CdS-3 photocatalyst has higher application value in the field of industrial wastewater treatment.
Experiment for photocatalytic degradation of other organic dyes
To further verify HNb3O8The photocatalytic performance of Au/CdS-3, the experiment, the HNb prepared3O8the/Au/CdS-3 is used as a photocatalyst to carry out experiments that other organic dyes have degradation effects, and the specific test objects are rhodamine B (RhB) and Methyl Orange (MO); the specific test method is the same as the method for degrading methylene blue by photocatalysis, and the change of the ultraviolet absorption spectrum is recorded.
FIGS. 7 and 8 respectively show the use of HNb3O8The UV absorption spectrum of RhB and MO degraded by the Au/CdS-3 photocatalyst in different treatment times. The curves in the figure are from top to bottom the results of the tests with the dye treated in the dark for 1 hour to the dye treated in the light for 6 hours. As can be seen from the figure, the absorbance of both solutions decreased significantly after 6 hours, indicating HNb3O8the/Au/CdS-3 photocatalyst has a good degradation effect on MB, has a certain degradation effect on organic dyes such as RhB and MO, and has a good application prospect in the field of industrial wastewater treatment containing various organic dyes.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A preparation method of a niobate composite nano material modified by CdS quantum dots is characterized by comprising the following steps:
a. preparing niobate nano sheets: mixing niobium ethoxide and triethanolamine to obtain a mixed solution I, adjusting the pH of the mixed solution I to be 12-13, reacting at 120-180 ℃ for 12-24 h to obtain colloidal suspension, removing precipitate, collecting light yellow supernatant colloid, centrifuging to obtain a solid product, washing and drying to obtain niobate nanosheets;
b. HNb3O8preparation of a/CdS composite material: b, mixing the niobate nanosheet and CdCl in the step a2、Na2S and cysteamine hydrochloride are dissolved in water to obtain a mixed solution II, the mixed solution II reacts for 5 to 10 hours at the temperature of 40 to 50 ℃ to obtain a yellow green suspension, the yellow green suspension is cooled to the room temperature, precipitate is separated, washed and dried to obtain a yellow solid product HNb3O8/CdS。
2. The method of claim 1, wherein the mass ratio of niobium ethoxide to triethanolamine in step a is 1: (2-10).
3. The method of claim 1, wherein the CdCl in step b is prepared by2With Na2The molar ratio of S is 1: (1-2); in the step b, the molar ratio of the niobate nanosheet to the CdS is 1 (1-5).
4. The niobate composite nanomaterial modified by CdS quantum dots prepared by the method of any one of claims 1-3.
5. A preparation method of niobate composite nanomaterial modified by Au nanoparticles and CdS quantum dots is characterized by comprising the following steps:
(1) preparing niobate nano sheets: mixing niobium ethoxide and triethanolamine to obtain a mixed solution I, adjusting the pH value of the mixed solution I to 12-13, reacting at the temperature of 120-180 ℃ for 12-24 hours to obtain a colloidal suspension, removing a precipitate, collecting a light yellow supernatant colloid, centrifuging to obtain a solid product, washing and drying to obtain a niobate nanosheet;
（2）HNb3O8preparing an Au/CdS composite material: dissolving the niobate flakes and chloroauric acid in the step (1) in water to obtain a mixed solution III, stirring and irradiating the mixed solution III for 30-60min to obtain a purple gray suspension, centrifuging, collecting a product, washing and drying to obtain Au-modified niobate flakes;
then adding the Au modified niobate nano-sheet and CdCl2、Na2S and cysteamine hydrochloride are dissolved in water to obtain a mixed solution IV, the mixed solution IV reacts for 5 to 10 hours at the temperature of 40 to 50 ℃ to obtain a yellow green suspension, the yellow green suspension is cooled to the room temperature, precipitate is separated, washed and dried to obtain a yellow green solid product HNb3O8/Au/CdS。
6. The method according to claim 5, wherein the mass ratio of niobium ethoxide to triethanolamine in step (1) is 1: (2-10).
7. The preparation method according to claim 5, wherein the mass ratio of the Au-modified niobate nanoplates to the cysteamine hydrochloride in step (2) is (0.3-1.6): 1.
8. The niobate composite nano material modified by Au nano particles and CdS quantum dots, which is prepared by the method of any one of claims 5 to 7.
9. Use of the composite nanomaterial of claim 4 or claim 8 as a photocatalyst in photocatalytic hydrogen production.
10. Use of the composite nanomaterial of claim 4 or claim 8 in degrading an artificial dye, wherein the artificial dye is rhodamine B, methylene blue, methyl orange, alizarin red S, or congo red.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210288080.XA CN114618527B (en) | 2022-03-23 | 2022-03-23 | Au nanoparticle and CdS quantum dot modified niobate composite nanomaterial and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210288080.XA CN114618527B (en) | 2022-03-23 | 2022-03-23 | Au nanoparticle and CdS quantum dot modified niobate composite nanomaterial and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114618527A true CN114618527A (en) | 2022-06-14 |
| CN114618527B CN114618527B (en) | 2023-05-23 |
Family
ID=81903814
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210288080.XA Active CN114618527B (en) | 2022-03-23 | 2022-03-23 | Au nanoparticle and CdS quantum dot modified niobate composite nanomaterial and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114618527B (en) |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2407419A1 (en) * | 2010-07-16 | 2012-01-18 | Universiteit Twente | Photocatalytic water splitting |
| CN104549263A (en) * | 2015-01-28 | 2015-04-29 | 福州大学 | Pd/niobate nanosheet catalyst as well as preparation method and application thereof |
| US20160367968A1 (en) * | 2013-10-24 | 2016-12-22 | Queen Mary University Of London | Photocatalysts |
| 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 |
| CN108607593A (en) * | 2016-01-26 | 2018-10-02 | 苏州大学 | Niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst of cadmium sulfide nano-particles modification and application |
| CN110227492A (en) * | 2019-04-29 | 2019-09-13 | 中国科学院山西煤炭化学研究所 | A kind of Nano semiconductor photochemical catalyst and preparation method thereof |
| JP2020025941A (en) * | 2018-08-17 | 2020-02-20 | 地方独立行政法人東京都立産業技術研究センター | Photocatalyst and method of manufacturing the same |
| US20200354235A1 (en) * | 2019-05-09 | 2020-11-12 | Soochow University | Heterojunction composite material consisting of one-dimensional in2o3 hollow nanotube and two-dimensional znfe2o4 nanosheet, and application thereof in water pollutant removal |
| CN112337457A (en) * | 2020-11-11 | 2021-02-09 | 郑州轻工业大学 | Mo-doped HNb3O8Preparation method and application of nanosheet |
| CN112928246A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | Composite material, preparation method and application thereof |
| CN113731497A (en) * | 2021-09-13 | 2021-12-03 | 福州大学 | CdS QDs loaded BPEI modified niobium pentoxide catalyst and preparation method and application thereof |
| CN113769763A (en) * | 2021-10-11 | 2021-12-10 | 陕西科技大学 | CdS-Au nano-catalyst and preparation method and application thereof |
-
2022
- 2022-03-23 CN CN202210288080.XA patent/CN114618527B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2407419A1 (en) * | 2010-07-16 | 2012-01-18 | Universiteit Twente | Photocatalytic water splitting |
| US20160367968A1 (en) * | 2013-10-24 | 2016-12-22 | Queen Mary University Of London | Photocatalysts |
| CN104549263A (en) * | 2015-01-28 | 2015-04-29 | 福州大学 | Pd/niobate nanosheet catalyst as well as preparation method and application thereof |
| CN108607593A (en) * | 2016-01-26 | 2018-10-02 | 苏州大学 | Niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst of cadmium sulfide nano-particles modification and application |
| 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 |
| JP2020025941A (en) * | 2018-08-17 | 2020-02-20 | 地方独立行政法人東京都立産業技術研究センター | Photocatalyst and method of manufacturing the same |
| CN110227492A (en) * | 2019-04-29 | 2019-09-13 | 中国科学院山西煤炭化学研究所 | A kind of Nano semiconductor photochemical catalyst and preparation method thereof |
| US20200354235A1 (en) * | 2019-05-09 | 2020-11-12 | Soochow University | Heterojunction composite material consisting of one-dimensional in2o3 hollow nanotube and two-dimensional znfe2o4 nanosheet, and application thereof in water pollutant removal |
| CN112928246A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | Composite material, preparation method and application thereof |
| CN112337457A (en) * | 2020-11-11 | 2021-02-09 | 郑州轻工业大学 | Mo-doped HNb3O8Preparation method and application of nanosheet |
| CN113731497A (en) * | 2021-09-13 | 2021-12-03 | 福州大学 | CdS QDs loaded BPEI modified niobium pentoxide catalyst and preparation method and application thereof |
| CN113769763A (en) * | 2021-10-11 | 2021-12-10 | 陕西科技大学 | CdS-Au nano-catalyst and preparation method and application thereof |
Non-Patent Citations (5)
| Title |
|---|
| DANDAN MA ET AL.: ""Au Nanoparticle and CdS Quantum Dot Codecoration of In2O3 Nanosheets for Improved H2 Evolution Resulting from Efficient Light Harvesting and Charge Transfer"", 《ACS SUSTAINABLE CHEMISTRY & ENGINEERING》 * |
| KEIZO NAKAGAWA ET AL.: ""Enhanced photocatalytic hydrogen evolution from water by niobate single molecular sheets and ensembles"", 《CHEMICAL COMMUNICATIONS》 * |
| MEIYING LIU ET AL.: ""Biomolecule-mediated hydrothermal synthesis of polyoxoniobate-CdS nanohybrids with enhanced photocatalytic performance for hydrogen production and RhB degradation"", 《DALTON TRANSACTIONS》 * |
| SHAOHUA SHEN ET AL.: ""Visible-light-driven photocatalytic water splitting on nanostructured semiconducting materials"", 《INTERNATIONAL JOURNAL OF NANOTECHNOLOGY》 * |
| 王冠: ""多铌、钽氧酸盐的合成、结构及性质研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114618527B (en) | 2023-05-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20210331149A1 (en) | Biochar-modified bismuth vanadate catalyst and preparation method and use thereof | |
| CN110918126B (en) | Preparation method of flower-shaped molybdenum disulfide combined UiO-66 photocatalyst | |
| CN108479759B (en) | Visible light response type lanthanum-doped bismuth tungstate catalyst and preparation method thereof | |
| CN106622322B (en) | It is a kind of using bimetal nano particles as two-dimensional nano piece composite photo-catalyst of hetero-junctions and preparation method thereof | |
| Cai et al. | Noble metal sandwich-like TiO2@ Pt@ C3N4 hollow spheres enhance photocatalytic performance | |
| CN111185210B (en) | Titanium carbide/titanium dioxide/black phosphorus nanosheet composite photocatalyst and preparation method and application thereof | |
| CN109317137B (en) | Hydrotalcite and bismuth molybdate heterojunction composite photocatalyst and preparation method and application thereof | |
| Sun et al. | Designing double Z-scheme heterojunction of g-C3N4/Bi2MoO6/Bi2WO6 for efficient visible-light photocatalysis of organic pollutants | |
| Zhao et al. | Novel carboxy-functionalized PVP-CdS nanopopcorns with homojunctions for enhanced photocatalytic hydrogen evolution | |
| CN112588283A (en) | Carbon quantum dot/mesoporous layered titanium dioxide and preparation method and application thereof | |
| CN111111734B (en) | Preparation and application of ferrous disulfide/carbon nitride composite photocatalyst | |
| CN110694627A (en) | Ferric oxide nano-ring photocatalyst and preparation method thereof | |
| CN112791729A (en) | Sulfhydrylation montmorillonite loaded ZnO-Fe2O3Heterojunction composite material and preparation method | |
| Zhu et al. | Cu-MOF modified Cd0. 5Zn0. 5S nanoparticles to form S-scheme heterojunction for efficient photocatalytic H2 evolution | |
| Wang et al. | Enhanced optical absorption and pollutant adsorption for photocatalytic performance of three-dimensional porous cellulose aerogel with BiVO4 and PANI | |
| Liu et al. | Photocatalytic activity study of ZnO modified with nitrogen–sulfur co-doped carbon quantum dots under visible light | |
| CN108568302B (en) | Opposite-symmetrical double-Z-shaped acoustic catalyst SnO2–CdSe–Bi2O3And preparation method and application thereof | |
| CN115845832B (en) | ZIF-8 derived ZnO/BiVO4Preparation method and application of heterojunction compound | |
| CN114618527B (en) | Au nanoparticle and CdS quantum dot modified niobate composite nanomaterial and application thereof | |
| CN111686763B (en) | Method for preparing magnetic zinc cadmium sulfide composite photocatalyst | |
| CN110075879B (en) | Carbon-coated ferroferric oxide magnetic microsphere modified bismuth oxyiodide composite photocatalytic material and preparation method and application thereof | |
| CN112619668A (en) | CdS @ SnS for photocatalysis2Composite material and preparation method and application thereof | |
| CN115646517B (en) | S mechanism Ni 11 (HPO 3 ) 8 (OH) 6 CdS heterojunction photocatalyst and preparation method thereof | |
| CN114471617B (en) | Magnetic photocatalyst, preparation method and application thereof | |
| Qi et al. | The photocatalytic properties and construction of a WS 2/MoS 2/CdS heterojunction |
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 |