CN106492841A - In2S3/NaTaO3The preparation method of compound nanometer photocatalyst - Google Patents
In2S3/NaTaO3The preparation method of compound nanometer photocatalyst Download PDFInfo
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- CN106492841A CN106492841A CN201610936926.0A CN201610936926A CN106492841A CN 106492841 A CN106492841 A CN 106492841A CN 201610936926 A CN201610936926 A CN 201610936926A CN 106492841 A CN106492841 A CN 106492841A
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- natao
- compound nanometer
- nanometer photocatalyst
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 29
- 150000001875 compounds Chemical class 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910003256 NaTaO3 Inorganic materials 0.000 claims abstract description 56
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000002114 nanocomposite Substances 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 6
- 229910002651 NO3 Inorganic materials 0.000 abstract description 4
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 abstract description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910001936 tantalum oxide Inorganic materials 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 239000004098 Tetracycline Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 229960002180 tetracycline Drugs 0.000 description 4
- 229930101283 tetracycline Natural products 0.000 description 4
- 235000019364 tetracycline Nutrition 0.000 description 4
- 150000003522 tetracyclines Chemical class 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to one kind prepares In with tantalum oxide, NaOH, indium nitrate and thioacetamide as raw material2S3/NaTaO3The method of compound nanometer photocatalyst, is a kind of preparation process is simple, and method with low cost, prepared compound nanometer photocatalyst have preferable photocatalytic activity.NaTaO is first weighed3, then weigh In (NO3)3·5H2O is put in beaker, is added deionized water, is uniformly mixing to obtain solution 1；Then weigh thioacetamide to add in solution 1, continue to be uniformly mixing to obtain suspension；Suspension is transferred in teflon-lined reactor, in 180 DEG C of constant temperature 12h, washing after natural cooling is dried to obtain In2S3/NaTaO3Nano-complex catalyst.
Description
Technical field
The present invention relates to one kind is with tantalum oxide (Ta2O5), NaOH (NaOH), indium nitrate (In (NO3)3·5H2) and sulphur O
For acetamide (CH3CSNH2) In is prepared for raw material2S3/NaTaO3The method of compound nanometer photocatalyst, is a kind of preparation technology
Simply, method with low cost, prepared compound nanometer photocatalyst have preferable photocatalytic activity.
Background technology
NaTaO3Therefore semiconductor exists as which is to environment nontoxicity, good stability and excellent photocatalytic activity
There are wide application, such as purification of air, hydrogen production by water decomposition and sewage purification etc. in environmental protection.However, it have wider
Band gap (Eg=4.0eV), can only respond to ultraviolet light, and ultraviolet light only accounts for the 4%-6% of sunshine, and visible ray is occupied
The significant proportion of sunshine.Therefore, it is necessary to be modified to which so which is to visible light-responded.In recent years, by two
Kind of semiconductor is ground so as to the absorption of light being extended to visible region from ultra-violet (UV) band becoming people building composite photocatalyst material
The focus that studies carefully.Another advantage of this method is to improve the transfer rate of electron-hole pair, reduces light induced electron and hole
Compound, so as to effectively improve the catalysis activity of compound.NaTaO by ultraviolet light response3Partly lead with visible light-responded
Body is combined, and can improve NaTaO3Separation of charge efficiency and enhancing photocatalytic activity.For example, K.Hemalata Reddy et al.
(Reddy K H,Martha S,Parida K M.Facile fabrication of Bi2O3/Bi-
NaTaO3photocatalysts for hydrogen generation under visible light irradiation
[J].RSC Advances,2012,2(25):9423-9436.) Bi is constructed2O3/Bi–NaTaO3Composite catalyst, it is seen that light
There is down excellent decomposition water H2-producing capacity；(Kumar S,Kumar B,Surendar T,et al.g-C3N4/
NaTaO3organic–inorganic hybrid nanocomposite:High-performance and recyclable
visible light driven photocatalyst[J].Materials Research Bulletin,2014,49:
310-318.) Santosh Kumar et al. are prepared for g-C3N4/NaTaO3Composite photo-catalyst；Xu et al. (Xu D, Shi W,
Song C,et al.In-situ synthesis and enhanced photocatalytic activity of
visible-light-driven plasmonic Ag/AgCl/NaTaO3nanocubes photocatalysts[J]
.Applied Catalysis B:Environmental,2016,191:228-234.) it is successfully prepared Ag/AgCl/NaTaO3
Composite, with preferable activity.
So far, it is not yet found that people prepares In2S3/NaTaO3Composite.The present invention is successfully prepared using hydro-thermal method
In2S3/NaTaO3Composite, prepared In2S3/NaTaO3Composite has applications well in fields such as environment, the energy
Prospect.
Content of the invention
It is an object of the present invention to provide a kind of use the synthetically prepared In of hydro-thermal method2S3/NaTaO3The side of compound nanometer photocatalyst
Method.
The present invention is realized by following steps：
NaTaO is first weighed3, then weigh In (NO3)3·5H2O is put in beaker, is added deionized water, is uniformly mixing to obtain
Solution 1；Then weigh thioacetamide to add in solution 1, continue to be uniformly mixing to obtain suspension；Suspension is transferred to poly- four
In the reactor of PVF liner, in 180 DEG C of constant temperature 12h, washing after natural cooling is dried to obtain In2S3/NaTaO3Nano combined
Thing catalyst.
The NaTaO3Mass volume ratio with deionized water is：1g：150mL.
The In2S3/NaTaO3In in nano-complex catalyst2S3Mass percent be：5%-40%.
Further, the In2S3/NaTaO3In in nano-complex catalyst2S3Mass percent be 20%.
The present invention is successfully prepared In using hydro-thermal method2S3/NaTaO3Compound nanometer photocatalyst, NaTaO3Vertical for nanometer
Box structure, the size of particle is 200-400nm, In2S3Nano-particles size is 10-15nm.
Using field emission scanning electron microscope (FESEM), x-ray photoelectron spectroscopy (XPS) and the ultraviolet suction of solid
Receive the instruments such as spectrum to be analyzed product, while photocatalytic degradation experiment is carried out with tetracycline as target antibiotic, lead to
Ultraviolet-visible spectrophotometer measurement absorbance is crossed, to assess its photocatalytic activity.
Description of the drawings
Fig. 1 is prepared In2S3/NaTaO3Compound nanometer photocatalyst field emission scanning electron microscope figure.
Fig. 2 is prepared In2S3/NaTaO3The XPS spectrum figure of compound nanometer photocatalyst.
Fig. 3 is prepared In2S3/NaTaO3The solid ultraviolet absorpting spectrum of compound nanometer photocatalyst.Wherein a is pure
NaTaO3, In in b2S3Account for the In2S3/NaTaO3Mass percent in nano-complex catalyst is In in 5%, c2S3
Account for the In2S3/NaTaO3Mass percent in nano-complex catalyst is In in 10%, d2S3Account for the In2S3/
NaTaO3Mass percent in nano-complex catalyst is In in 20%, e2S3Account for the In2S3/NaTaO3Nano-complex
Mass percent in catalyst is pure In for 30%, f2S3.
Fig. 4 is that prepared difference contains In2S3/NaTaO3Compound nanometer photocatalyst Visible Light Induced Photocatalytic tetracycline activity figure.
Wherein a is pure In2S3, In in b2S3Account for the In2S3/NaTaO3Mass percent in nano-complex catalyst is 5%,
In in c2S3Account for the In2S3/NaTaO3Mass percent in nano-complex catalyst is In in 40%, d2S3Account for described
In2S3/NaTaO3It is middle In that mass percent in nano-complex catalyst is 10%, e2S3Account for the In2S3/NaTaO3Receive
Mass percent in rice complex catalyst is In in 30%, f2S3Account for the In2S3/NaTaO3In nano-complex catalyst
Mass percent be 20%.
Specific embodiment
1 In of embodiment2S3/NaTaO3The preparation of compound nanometer photocatalyst
(1) 0.221g Ta are weighed respectively2O5With 0.6g NaOH, it is added in 50mL reactors, adds 30mL deionizations
Solution stirring 10min is well mixed which, the solution of acquisition is transferred to teflon-lined reactor then by water
In, in 140 DEG C of constant temperature 12h, then after natural cooling, obtain a cube block-shaped NaTaO3.
(2) 0.2g NaTaO are weighed3, then weigh a certain amount of In (NO3)3·5H2O is put in beaker, add 30mL go from
Sub- water, stirs 1h；Then certain thioacetamide is added in above-mentioned solution, continues stirring 1h, and the suspension of gained is transferred to
In teflon-lined reactor, in 180 DEG C of constant temperature 12h, washing after natural cooling is dried to obtain product.
2 In of embodiment2S3/NaTaO3The sign of compound nanometer photocatalyst
As shown in figure 1, In2S3/NaTaO3As can be seen that In in the field emission scanning electron microscope of compound nanometer photocatalyst2S3
Nano-particle has been compound to NaTaO well3Cubic block surface, NaTaO3The size of cubic block is in 200-300nm.
As shown in Fig. 2 it can be seen that there is the presence of S, In, O, Ta, Na element in XPS figures.
As shown in figure 3, In2S3/NaTaO3As can be seen that pure in the solid ultra-violet absorption spectrum of compound nanometer photocatalyst
NaTaO3There is stronger response in ultraviolet region, it is seen that light area does not absorb substantially, with In2S3After carrying out being combined, which is in visible ray
There is in spectral limit stronger response, and with In2S3The increase of content, absorbs and gradually strengthens.
The In of 3 different content of embodiment2S3/NaTaO3The visible light catalysis activity experiment of composite photo-catalyst
(1) compound concentration is the tetracycline of 100mg/L, and the solution for preparing is placed in dark place.
(2) In of different content is weighed2S3/NaTaO3Surface recombination photochemical catalyst 50mg, is respectively placed in photo catalysis reactor
In, the target degradation solution prepared by addition 100mL steps (1), after magnetic agitation 60min photochemical catalyst to be composite is uniformly dispersed,
Light source is opened, condensation water is connected, is carried out photocatalytic degradation experiment.
(3) the photocatalytic degradation liquid 5mL in reactor is drawn per 30min, through being centrifuged off measuring which is ultraviolet after catalyst-
Visible absorbance.
(4) nano composite photo-catalyst prepared as seen from Figure 4 has excellent visible light catalysis activity, especially
In2S3Content be that 20% sample shows best degrading activity, with pure In2S3Compare, the drop of tetracycline in 180min
Solution activity about improves 2 times.
Claims (5)
1.In2S3/NaTaO3The preparation method of compound nanometer photocatalyst, it is characterised in that：NaTaO is first weighed3, then weigh In
(NO3)3·5H2O is put in beaker, is added deionized water, is uniformly mixing to obtain solution 1；Then it is molten that thioacetamide addition is weighed
In liquid 1, continue to be uniformly mixing to obtain suspension；Suspension is transferred in teflon-lined reactor, in 180 DEG C of perseverances
Warm 12h, washing after natural cooling are dried to obtain In2S3/NaTaO3Nano-complex catalyst.
2. In as claimed in claim 12S3/NaTaO3The preparation method of compound nanometer photocatalyst, it is characterised in that：Described
NaTaO3Mass volume ratio with deionized water is：1g：150mL.
3. In as claimed in claim 12S3/NaTaO3The preparation method of compound nanometer photocatalyst, it is characterised in that：Described
In2S3/NaTaO3In in nano-complex catalyst2S3Mass percent be：5%-40%.
4. In as claimed in claim 32S3/NaTaO3The preparation method of compound nanometer photocatalyst, it is characterised in that：Described
In2S3/NaTaO3In in nano-complex catalyst2S3Mass percent be 20%.
5. In as claimed in claim 12S3/NaTaO3The preparation method of compound nanometer photocatalyst, it is characterised in that：Described
In2S3/NaTaO3Compound nanometer photocatalyst, NaTaO3For nano cubic block structure, the size of particle is 200-400nm,
In2S3Nano-particles size is 10-15nm；In2S3Nanocomposites have arrived NaTaO3Cubic block surface.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108126718A (en) * | 2017-12-25 | 2018-06-08 | 江苏大学 | A kind of In2S3/BiPO4The preparation method and applications of heterojunction photocatalyst |
| CN114558591A (en) * | 2022-02-18 | 2022-05-31 | 复旦大学 | Ternary Au/ZnIn2S4/NaTaO3Nano-cube composite photocatalyst and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101961655A (en) * | 2010-08-30 | 2011-02-02 | 天津工业大学 | Indium sulfide photocatalyst with visible light response and preparation method thereof |
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2016
- 2016-10-25 CN CN201610936926.0A patent/CN106492841B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101961655A (en) * | 2010-08-30 | 2011-02-02 | 天津工业大学 | Indium sulfide photocatalyst with visible light response and preparation method thereof |
Non-Patent Citations (4)
| Title |
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| CHAOSHENG XING,ET.AL.: "Hydrothermal synthesis of In2S3/g-C3N4 heterojunctions with enhanced photocatalytic activity", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
| XIA LI,ET.AL.: "Facile Hydrothermal Synthesis of Sodium Tantalate (NaTaO3) Nanocubes and High Photocatalytic Properties", 《J. PHYS. CHEM. C》 * |
| 何杰 等: "《工业催化》", 31 July 2014, 中国矿业大学出版社 * |
| 孟越: "CdS-NaTaO3复合型光催化剂的制备及光降解污染物研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108126718A (en) * | 2017-12-25 | 2018-06-08 | 江苏大学 | A kind of In2S3/BiPO4The preparation method and applications of heterojunction photocatalyst |
| CN114558591A (en) * | 2022-02-18 | 2022-05-31 | 复旦大学 | Ternary Au/ZnIn2S4/NaTaO3Nano-cube composite photocatalyst and preparation method and application thereof |
| CN114558591B (en) * | 2022-02-18 | 2023-10-03 | 复旦大学 | Ternary Au/ZnIn 2 S 4 /NaTaO 3 Nano cube composite photocatalyst, preparation method and application thereof |
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