CN106492841B - In2S3/NaTaO3The preparation method of compound nanometer photocatalyst - Google Patents
In2S3/NaTaO3The preparation method of compound nanometer photocatalyst Download PDFInfo
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- CN106492841B CN106492841B CN201610936926.0A CN201610936926A CN106492841B CN 106492841 B CN106492841 B CN 106492841B CN 201610936926 A CN201610936926 A CN 201610936926A CN 106492841 B CN106492841 B CN 106492841B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 27
- 150000001875 compounds Chemical class 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 229910003256 NaTaO3 Inorganic materials 0.000 claims abstract description 55
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000725 suspension Substances 0.000 claims abstract description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000002105 nanoparticle Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 claims description 2
- 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 7
- 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 6
- 239000004098 Tetracycline Substances 0.000 description 4
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 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
- 238000006555 catalytic reaction 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
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 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
- 239000002114 nanocomposite Substances 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
- 238000012546 transfer Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000010521 absorption reaction 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
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004140 cleaning Methods 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
- 238000002242 deionisation method Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000746 purification 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
- 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)
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Abstract
The present invention relates to one kind to prepare In as raw material using tantalum oxide, sodium hydroxide, indium nitrate and thioacetamide2S3/NaTaO3The method of compound nanometer photocatalyst is that a kind of preparation process is simple, low-cost method, and prepared compound nanometer photocatalyst has preferable photocatalytic activity.First weigh NaTaO3, then weigh In (NO3)3·5H2O is put in beaker, and deionized water is added, is uniformly mixing to obtain solution 1；Then it weighs thioacetamide to be added in solution 1, continues to be uniformly mixing to obtain suspension；Suspension is transferred in the reaction kettle of polytetrafluoroethyllining lining, washing is dried to obtain In after 180 DEG C of constant temperature 12h, natural cooling2S3/NaTaO3Nano-complex catalyst.
Description
Technical field
The present invention relates to one kind with tantalum oxide (Ta2O5), sodium hydroxide (NaOH), indium nitrate (In (NO3)3·5H2O) and
Thioacetamide (CH3CSNH2) it is raw material to prepare In2S3/NaTaO3The method of compound nanometer photocatalyst is a kind of to prepare work
Skill is simple, low-cost method, and prepared compound nanometer photocatalyst has preferable photocatalytic activity.
Background technique
NaTaO3Semiconductor is since it is non-toxic to environment, good stability and excellent photocatalytic activity, therefore
There are wide application, such as air cleaning, hydrogen production by water decomposition and sewage purification etc. in environmental protection.However, it possess it is wider
Band gap (Eg=4.0eV), can only respond ultraviolet light, and ultraviolet light only accounts for the 4%-6% of sunlight, and visible light occupies
The significant proportion of sunlight.Therefore, it is necessary to modification be carried out to it to make it to visible light-responded.In recent years, pass through two
Kind of semiconductor constructs composite photocatalyst material, grinds so that the absorption of light from ultra-violet (UV) band is extended to visible region and becomes people
The hot spot studied carefully.Another advantage of this method is to improve the transfer rate of electron-hole pair, reduces light induced electron and hole
It is compound, thus effectively improve compound catalytic activity.By the NaTaO of ultraviolet light response3It is partly led with visible light-responded
Body progress is compound, 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.) construct Bi2O3/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. is 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 material has preferable activity.
So far, it is not yet found that people prepares In2S3/NaTaO3Composite material.The present invention is successfully prepared using hydro-thermal method
In2S3/NaTaO3Composite material, prepared In2S3/NaTaO3Composite material has applications well in fields such as environment, the energy
Prospect.
Summary of the invention
In is synthetically prepared using hydro-thermal method it is an object of the present invention to provide a kind of2S3/NaTaO3The side of compound nanometer photocatalyst
Method.
The present invention is realized by following steps:
First weigh NaTaO3, then weigh In (NO3)3·5H2O is put in beaker, and deionized water is added, is uniformly mixing to obtain
Solution 1；Then it weighs thioacetamide to be added in solution 1, continues to be uniformly mixing to obtain suspension；Suspension is transferred to poly- four
In the reaction kettle of vinyl fluoride liner, washing is dried to obtain In after 180 DEG C of constant temperature 12h, natural cooling2S3/NaTaO3It is nano combined
Object catalyst.
The NaTaO3With the mass volume ratio of deionized water are as follows: 1g:150mL.
The In2S3/NaTaO3In in nano-complex catalyst2S3Mass percent are as follows: 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, NaTaO3It is vertical for nanometer
Box structure, the size of particle are 200-400nm, In2S3Nano-particles size is 10-15nm.
It is inhaled using outside field emission scanning electron microscope (FESEM), x-ray photoelectron spectroscopy (XPS) and solid violet
It receives the instruments such as spectrum to analyze product, while carrying out photocatalytic degradation experiment by target antibiotic of tetracycline, lead to
Ultraviolet-visible spectrophotometer measurement absorbance is crossed, to assess its photocatalytic activity.
Detailed description of the invention
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 that 30%, f is pure In2S3。
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%, d2S3It accounts for described
In2S3/NaTaO3Mass percent in nano-complex catalyst is that 10%, e is middle In2S3Account for the In2S3/NaTaO3It receives
Mass percent in rice complex catalyst is In in 30%, f2S3Account for the In2S3/NaTaO3Nano-complex catalyst
In mass percent be 20%.
Specific embodiment
1 In of embodiment2S3/NaTaO3The preparation of compound nanometer photocatalyst
(1) 0.221g Ta is weighed respectively2O5It with 0.6g NaOH, is added in 50mL reaction kettle, 30mL deionization is added
Solution stirring 10min is uniformly mixed it, then the solution of acquisition is transferred to the reaction kettle of polytetrafluoroethyllining lining 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 is weighed3, then weigh a certain amount of In (NO3)3·5H2O is put in beaker, and 30mL is added and goes
Ionized water stirs 1h；Then certain thioacetamide is added in above-mentioned solution, continues to stir 1h, resulting suspension transfer
Into the reaction kettle of polytetrafluoroethyllining lining, washing is dried to obtain product after 180 DEG C of constant temperature 12h, natural cooling.
2 In of embodiment2S3/NaTaO3The characterization 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
Nanoparticle has been combined 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 figure.
As shown in figure 3, In2S3/NaTaO3It is in the solid ultra-violet absorption spectrum of compound nanometer photocatalyst as can be seen that pure
NaTaO3There is stronger response in ultraviolet region, it is seen that light area does not absorb substantially, with In2S3Carry out it is compound after, in visible light
There is stronger response, and with In in spectral limit2S3The increase of content, absorption gradually increase.
The In of 3 different content of embodiment2S3/NaTaO3The visible light catalysis activity of composite photo-catalyst is tested
(1) compound concentration is the tetracycline of 100mg/L, and the solution prepared 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 that 100mL step (1) is prepared is added, after magnetic agitation 60min photochemical catalyst to be composite is uniformly dispersed,
Light source is opened, condensation water is connected, carries out photocatalytic degradation experiment.
(3) every 30min draws the photocatalytic degradation liquid 5mL in reactor, measure that its is ultraviolet after being centrifuged off catalyst-
Visible absorbance.
(4) prepared nano composite photo-catalyst has excellent visible light catalysis activity as seen from Figure 4, especially
In2S3Content be 20% sample show best degrading activity, with pure In2S3It compares, tetracycline in 180min
Degrading activity about improves 2 times.
Claims (3)
1.In2S3/NaTaO3The preparation method of compound nanometer photocatalyst, it is characterised in that: first weigh NaTaO3, then weigh In
(NO3)3·5H2O is put in beaker, and deionized water is added, is uniformly mixing to obtain solution 1；Then it is molten to weigh thioacetamide addition
In liquid 1, continue to be uniformly mixing to obtain suspension；Suspension is transferred in the reaction kettle of polytetrafluoroethyllining lining, in 180 DEG C of perseverances
Warm 12h, washing is dried to obtain In after natural cooling2S3/NaTaO3Nano-complex catalyst.
2. In as described in claim 12S3/NaTaO3The preparation method of compound nanometer photocatalyst, it is characterised in that: described
In2S3/NaTaO3In in nano-complex catalyst2S3Mass percent are as follows: 5%, 10%, 20%, 30%, 40%.
3. In as described 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；In2S3Nanoparticle during formation growth in situ to NaTaO3Nano cubic
Block surface.
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