CN106345494B - A kind of efficient visible light degradation agent nano-sheet In2.77S4Preparation method - Google Patents
A kind of efficient visible light degradation agent nano-sheet In2.77S4Preparation method Download PDFInfo
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- CN106345494B CN106345494B CN201610896614.1A CN201610896614A CN106345494B CN 106345494 B CN106345494 B CN 106345494B CN 201610896614 A CN201610896614 A CN 201610896614A CN 106345494 B CN106345494 B CN 106345494B
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- 230000015556 catabolic process Effects 0.000 title claims abstract description 40
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000002135 nanosheet Substances 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 229910001449 indium ion Inorganic materials 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- YZZFBYAKINKKFM-UHFFFAOYSA-N dinitrooxyindiganyl nitrate;hydrate Chemical compound O.[In+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZZFBYAKINKKFM-UHFFFAOYSA-N 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [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 abstract description 15
- 229940043267 rhodamine b Drugs 0.000 abstract description 15
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 abstract description 13
- 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 abstract description 10
- 229940012189 methyl orange Drugs 0.000 abstract description 10
- 230000000694 effects Effects 0.000 description 13
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 6
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 239000005864 Sulphur Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000005286 illumination Methods 0.000 description 5
- 229910052738 indium Inorganic materials 0.000 description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000002994 raw material Substances 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
- 238000001035 drying Methods 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 3
- 241000446313 Lamella Species 0.000 description 3
- 229960001484 edetic acid Drugs 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- PWKSKIMOESPYIA-UHFFFAOYSA-N 2-acetamido-3-sulfanylpropanoic acid Chemical compound CC(=O)NC(CS)C(O)=O PWKSKIMOESPYIA-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 1
Classifications
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- 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
-
- 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
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Toxicology (AREA)
- Thermal Sciences (AREA)
- Health & Medical Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Physical Water Treatments (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of efficient visible light degradation agent nano-sheet In2.77S4Preparation method, include the following steps：A, it stocks up：Take In (NO3)3·4.5H2O, thioacetamide is completely dissolved in deionized water, wherein the mol ratio of a concentration of 0.05mol/L of indium ion, indium ion and sulphion are 1:3‑1:5, be placed in the hydrothermal reaction kettle of inner liner polytetrafluoroethylene；B, it reacts：It is 180 DEG C to control hydrothermal temperature, and the reaction time is 14 16 hours, waits for reaction kettle cooled to room temperature after reaction；C, it post-processes：By in reaction kettle product take out, wash repeatedly with deionized water, filter to neutrality after dry, obtain sheet In2.77S4.The method of the present invention is simple, reaction condition is mild, technological process is short, preparation efficiency is high, and products obtained therefrom is high to the degradation efficiency of rhodamine B, methyl orange, potassium bichromate under visible light.
Description
Technical field
The invention belongs to photodegradable aid field of material technology, are related to a kind of preparation method of photodegradable aid, specifically
Efficient visible light degradation agent nano-sheet In2.77S4Preparation method.
Background technology
The pollution problem of organic matter and heavy metal in water body is always to perplex the great difficult problem of the mankind, the birth of photodegradable aid
The raw dawn that " green, environmental protection " is provided to solve this problem, but traditional photodegradable aid such as TiO2, ZnO etc., energy gap
More than 2.9eV, greater band gap is insensitive to visible light and infrared light, only has preferable degradation effect under ultraviolet light, and purple
Outer light accounting in entire sunlight is only 5% or so.Therefore, it improves the disposal efficiency, obtain the efficiency light drop under visible light
Solution agent becomes world's hot spot in recent years.It is generally acknowledged that：Substance of the energy gap less than 2.9eV has preferable under visible light
Response range.Based on this, energy gap becomes an important indicator for weighing photodegradable aid photoresponse degree.Metal vulcanizes
The energy gap of object is less than 2.9eV mostly, and many scholars have made a large amount of research to the series compound, obtain it is a series of can
The achievement of happiness has significantly pushed the development in light degradation field.Such as：Luo et al. is with SnCl4·5H2O is raw material with thiocarbamide, uses water
Hot method has synthesized lamella SnS2, the energy gap of the material is 2.1eV, the methyl orange of 60min degradable 35%；Yang et al. with
ZnCl2、InCl3·4H2O, thioacetamide is raw material, with solvent structure lamella ZnIn2S4, the energy gap of the material
For 2.17eV, the methyl orange of 70min degradable 95%；Han et al. is with InCl3, L-cysteine, polyethylene glycol, polystyrene
Sodium sulfonate is raw material, and petal-shaped In has been synthesized with hydro-thermal method2S3, the energy gap of the material is 2.0eV, 60min degradable 90%
2,4- chlorophenesic acids；It is worth noting that：Wang et al. is in CN102335616 with InCl3·4H2O and thioacetamide are
Raw material has synthesized the In of bouquet shape with hydro-thermal method2S3, degradable 90% methyl orange in 2.5h of the material, with preferable
Practical function.But the synthetic method of above-mentioned degradation agent is more complex, technological process is long, and preparation efficiency is low.And how existing
Have in technical foundation, research and development one kind can further increase degradation effect, and method is simple, and technological process is short, and preparation efficiency is high
Visible Light Induced Photocatalytic agent material is the target that we research and develop.
Invention content
The present invention is to comply with above-mentioned R＆D target, devises a kind of efficient visible light degradation agent nano-sheet In2.77S4's
Preparation method, this method is simple, reaction condition is mild, technological process is short, preparation efficiency is high and the energy gap of the product of synthesis
It is small, there is excellent photoresponse effect under visible light.
The technical solution adopted by the present invention is a kind of efficient visible light degradation agent nano-sheet In2.77S4Preparation method,
Include the following steps：
A, it stocks up：
Indium nitrate hydrate, thioacetamide is taken to be completely dissolved in deionized water, wherein indium ion is a concentration of
The mol ratio of 0.05mol/L, indium ion and sulphion are 1:3-1:5, the hydro-thermal reaction for being placed on inner liner polytetrafluoroethylene
In kettle；
B, it reacts：
It is 180 DEG C to control hydrothermal temperature, and the reaction time is 14-16 hours, waits for that reaction kettle is naturally cold after reaction
But to room temperature；
C, it post-processes：
By in reaction kettle product take out, wash repeatedly with deionized water, filter to neutrality after dry, to obtain sheet
In2.77S4。
The indium nitrate hydrate is In (NO3)3·4.5H2O。
Sheet In obtained by step C2.77S4Thickness be 5-20nm.
Preferably, the sheet In obtained by step C2.77S4Thickness be 10nm.
The beneficial effects of the invention are as follows：Raw material is adjusted, indium nitrate hydrate, thioacetamide are completely dissolved in deionization
In water, control indium ion and sulphion mol ratio, be placed in the hydrothermal reaction kettle of inner liner polytetrafluoroethylene, pass through control
Reaction time processed and temperature, a step Fast back-projection algorithm go out efficient visible light degradation agent nano-sheet In2.77S4, the forbidden band of the product is wide
Spend it is small, under visible light have excellent photoresponse effect, be at present reported the substance best to rhodamine B degradation effect it
One, while the product is high to methyl orange and potassium bichromate degradation efficiency, to solving the dirt of organic matter and heavy metal in water pollution
Dye problem has significant reference and wide application prospect.
Description of the drawings
Fig. 1 is the transmission electron microscope figure of product in embodiment 2.
Fig. 2 is the X-ray diffractogram of product in embodiment 2.
Fig. 3 be embodiment 2 in product it is ultraviolet-diffuse spectrogram.
Fig. 4 is the degradation effect figure of product under visible light in embodiment 2.
Fig. 5 is the degradation effect figure that product adds different sacrifice agents under visible light in embodiment 2.
Specific implementation mode
Invention is described further in the following with reference to the drawings and specific embodiments：
Embodiment 1
1, appropriate In (NO are weighed3)3·4.5H2O (Sinopharm Chemical Reagent Co., Ltd., similarly hereinafter), thioacetamide
(Sinopharm Chemical Reagent Co., Ltd., similarly hereinafter) be completely dissolved in deionized water, be placed on inner liner polytetrafluoroethylene
In hydrothermal reaction kettle；Wherein, the mol ratio of a concentration of 0.05mol/L of indium ion, indium and sulphur is 1:3.
2, control hydrothermal temperature be 180 DEG C, reaction time 14h, after reaction reaction kettle naturally cool to room
Temperature.
3, the product in step 2 is taken out from reaction kettle, washs drying after suction filtration to neutrality repeatedly with deionized water, obtains
To the powder In that lamellar spacing is 5nm2.77S4。
4, the In of 0.05g is weighed2.77S4It is molten to be respectively placed in 10mg/L rhodamine B solutions, the methyl orange of 10mg/L for product
Liquid, 70mg/L potassium bichromate solution in, 300W xenon lamp irradiation under carry out photocatalytic degradation experiment, adopted in illumination
Ultraviolet light is filtered off with optical filter.The experimental results showed that the In obtained under this condition2.77S4It degrades to rhodamine B solution in 9min
Rate reaches the degradation rate of potassium bichromate solution up to 87%, in 60min up to 98%, in 30min to the degradation rate of methyl orange solution
86%.
Embodiment 2
1, appropriate In (NO are weighed3)3·4.5H2O, thioacetamide is completely dissolved in deionized water, be placed on liner
In the hydrothermal reaction kettle of polytetrafluoroethylene (PTFE)；Wherein, the mol ratio of a concentration of 0.05mol/L of indium ion, indium and sulphur is 1:4.
2, control hydrothermal temperature be 180 DEG C, reaction time 15h, after reaction reaction kettle naturally cool to room
Temperature.
3, the product in step 2 is taken out from reaction kettle, washed repeatedly with deionized water, filter to neutrality after it is dry,
Obtain the powder In that lamellar spacing is 10nm2.77S4。
4, the In of 0.05g is weighed2.77S4It is molten to be respectively placed in 10mg/L rhodamine B solutions, the methyl orange of 10mg/L for product
Liquid, 70mg/L potassium bichromate solution in, 300W xenon lamp irradiation under carry out photocatalytic degradation experiment, adopted in illumination
Ultraviolet light is filtered off with optical filter.The experimental results showed that the In obtained under this condition2.77S4It degrades to rhodamine B solution in 9min
Rate up to 99.9%, in 30min to the degradation rate of methyl orange solution up to 88%, in 60min to the degradation rate of potassium bichromate solution
Up to 87%.
Fig. 1 descriptions are the transmission electron microscope figure of product, and as can be seen from Figure, the pattern of products obtained therefrom is sheet knot
The thickness of structure, lamella is 10nm；Fig. 2 descriptions are the X-ray diffractogram of product, from figure it is found that the characteristic diffraction peak 2 of the product
θ is 23.435 °, 27.553 °, 28.804 °, 33.381 °, 43.813 °, 47.929 °, 56.177 °, 59.663 ° and 70.116 °,
With In2.77S4Base peak (PDF#88-2495) unanimously, the indices of crystallographic plane correspond respectively to (220), (311), (222), (400),
(511)、(440)、(533)、(444)、(800)；Fig. 3 description be product it is ultraviolet-diffuse spectrogram, can from figure
Go out, In2.77S4It is wider to the response range of visible light, to visible light-responded apparent, energy gap 1.75eV, hence it is evident that be less than
2.9eV is currently reported minimum one of energy gap；Fig. 4 descriptions are the degradation effect figure of product under visible light,
As can be seen from Figure, In2.77S4In 9min to rhodamine B solution degradation rate up to 99.9%, in 30min to methyl orange solution
Degradation rate up to 88%, in 60min to the degradation rate of potassium bichromate solution up to 87%, fully show the product have excellent drop
Effect is solved, and there is effect simultaneously to gas chromatography/heavy metal.Fig. 5 is that product adds difference under visible light in embodiment 2
The degradation effect figure of sacrifice agent, the figure can reflect that the light degradation mechanism of product, concrete operations are as follows：Weigh 0.05g In2.77S4
Product is placed in 10mg/L rhodamine B solutions, and sacrifice agent is added before adding light source, and later step is identical as step 4, sacrificial
Domestic animal agent is ethylenediamine tetra-acetic acid or sodium bicarbonate.Experimental result shows that the light degradation effect before and after ethylenediamine tetra-acetic acid is added in comparison
Fruit, product become 90% to the degradation rate of rhodamine B solution in 9min from 99.9%, this illustrates that light drops in ethylenediamine tetra-acetic acid
Solution inhibits to be not obvious, that is, hole is smaller to photodegradative effect；And after sodium bicarbonate is added, product is in 9min to Luo Dan
The degradation rate of bright B solution becomes 30% from 99.9%, this illustrates that sodium bicarbonate has significantly inhibiting effect to light degradation, that is,
Electronics plays a leading role during photodegradative.
Embodiment 3
1, appropriate In (NO are weighed3)3·4.5H2O, thioacetamide is completely dissolved in deionized water, be placed on liner
In the hydrothermal reaction kettle of polytetrafluoroethylene (PTFE)；Wherein, the mol ratio of a concentration of 0.05mol/L of indium ion, indium and sulphur is 1:5.
2, control hydrothermal temperature be 180 DEG C, reaction time 14h, after reaction reaction kettle naturally cool to room
Temperature.
3, the product in step 2 is taken out from reaction kettle, washs drying after suction filtration to neutrality repeatedly with deionized water, obtains
To the powder In that lamellar spacing is 20nm2.77S4。
4, the In of 0.05g is weighed2.77S4It is molten to be respectively placed in 10mg/L rhodamine B solutions, the methyl orange of 10mg/L for product
Liquid, 70mg/L potassium bichromate solution in, 300W xenon lamp irradiation under carry out photocatalytic degradation experiment, adopted in illumination
Ultraviolet light is filtered off with optical filter.The experimental results showed that the In obtained under this condition2.77S4It degrades to rhodamine B solution in 9min
Rate reaches the degradation rate of potassium bichromate solution up to 85%, in 60min up to 93%, in 30min to the degradation rate of methyl orange solution
86%.
Example 4：
1, appropriate In (NO are weighed3)3·4.5H2O, thioacetamide is completely dissolved in deionized water, be placed on liner
In the hydrothermal reaction kettle of polytetrafluoroethylene (PTFE)；Wherein, the mol ratio of a concentration of 0.05mol/L of indium ion, indium and sulphur is 1:3.
2, control hydrothermal temperature be 180 DEG C, reaction time 16h, after reaction reaction kettle naturally cool to room
Temperature.
3, the product in step 2 is taken out from reaction kettle, washs drying after suction filtration to neutrality repeatedly with deionized water, obtains
To the powder In that lamellar spacing is 16nm2.77S4。
4, the In of 0.05g is weighed2.77S4It is molten to be respectively placed in 10mg/L rhodamine B solutions, the methyl orange of 10mg/L for product
Liquid, 70mg/L potassium bichromate solution in, 300W xenon lamp irradiation under carry out photocatalytic degradation experiment, adopted in illumination
Ultraviolet light is filtered off with optical filter.The experimental results showed that the In obtained under this condition2.77S4It degrades to rhodamine B solution in 9min
Rate reaches the degradation rate of potassium bichromate solution up to 83%, in 60min up to 94%, in 30min to the degradation rate of methyl orange solution
84%.
Example 5：
1, appropriate In (NO are weighed3)3·4.5H2O, thioacetamide is completely dissolved in deionized water, be placed on liner
In the hydrothermal reaction kettle of polytetrafluoroethylene (PTFE)；Wherein, the mol ratio of a concentration of 0.05mol/L of indium ion, indium and sulphur is 1:4.
2, control hydrothermal temperature be 180 DEG C, reaction time 16h, after reaction reaction kettle naturally cool to room
Temperature.
3, the product in step 2 is taken out from reaction kettle, washs drying after suction filtration to neutrality repeatedly with deionized water, obtains
To the powder In that lamellar spacing is 7nm2.77S4。
4, the In of 0.05g is weighed2.77S4It is molten to be respectively placed in 10mg/L rhodamine B solutions, the methyl orange of 10mg/L for product
Liquid, 70mg/L potassium bichromate solution in, 300W xenon lamp irradiation under carry out photocatalytic degradation experiment, adopted in illumination
Ultraviolet light is filtered off with optical filter.The experimental results showed that the In obtained under this condition2.77S4It degrades to rhodamine B solution in 9min
Rate reaches the degradation rate of potassium bichromate solution up to 88%, in 60min up to 98%, in 30min to the degradation rate of methyl orange solution
87%.
Claims (4)
1. a kind of efficient visible light degradation agent nano-sheet In2.77S4Preparation method, it is characterised in that：The method and step
Include：
A, it stocks up：
Indium nitrate hydrate, thioacetamide is taken to be completely dissolved in deionized water, wherein a concentration of 0.05mol/L of indium ion,
The mol ratio of indium ion and sulphion is 1:3-1:5, be placed in the hydrothermal reaction kettle of inner liner polytetrafluoroethylene；
B, it reacts：
It is 180 DEG C to control hydrothermal temperature, and the reaction time is 14-16 hours, waits for that reaction kettle naturally cools to after reaction
Room temperature；
C, it post-processes：
By in reaction kettle product take out, wash repeatedly with deionized water, filter to neutrality after dry, to obtain sheet
In2.77S4。
2. a kind of efficient visible light degradation agent nano-sheet according to claim 12.77S4Preparation method, feature
It is：The indium nitrate hydrate is In (NO3)3·4.5H2O。
3. a kind of efficient visible light degradation agent nano-sheet according to claim 12.77S4Preparation method, feature
It is：Sheet In obtained by step C2.77S4Thickness be 5-20nm.
4. a kind of efficient visible light degradation agent nano-sheet according to claim 32.77S4Preparation method, feature
It is：Sheet In obtained by step C2.77S4Thickness be 10nm.
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Citations (3)
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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 |
| CN104588039A (en) * | 2014-12-31 | 2015-05-06 | 山东玉皇新能源科技有限公司 | Indium sulfide photocatalyst with hierarchical structures and preparation method thereof |
| CN104959151A (en) * | 2015-06-02 | 2015-10-07 | 福州大学 | Indium sulfide catalyst and its preparation method and use |
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Patent Citations (3)
| 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 |
| CN104588039A (en) * | 2014-12-31 | 2015-05-06 | 山东玉皇新能源科技有限公司 | Indium sulfide photocatalyst with hierarchical structures and preparation method thereof |
| CN104959151A (en) * | 2015-06-02 | 2015-10-07 | 福州大学 | Indium sulfide catalyst and its preparation method and use |
Non-Patent Citations (4)
| Title |
|---|
| "An In2.77S4@conductive carbon composite with superior electrocatalytic activity for dye-sensitized solar cells";Mingxing Guo et al;《Journal of photochemistry and photobiology a: chemistry》;20160728;第332卷;第87-91页 * |
| "Novel b-In2.77S4 nanosheet-assembled hierarchical microspheres: synthesis and high performance for photocatalytic reduction of Cr(VI)";Leqiang Shao et al;《The Royal Society of Chemistry》;20160205;第6卷;第18227-18234页 * |
| "Solar photocatalytic activity of indium sulfide nanocrystal and degradation of the tetracycline by In2S3";Cuiling Ai et al;《Desalination and Water Treatment》;20151215;第1-9页 * |
| "硫化物催化材料的合成及在染料敏化太阳能电池中的应用";姜维;《万方数据知识服务平台》;20151102;第28页 * |
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