CN106345494A - Preparation method of high-efficiency visible light degradation agent nanosheet In2.77S4 - Google Patents
Preparation method of high-efficiency visible light degradation agent nanosheet In2.77S4 Download PDFInfo
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- CN106345494A CN106345494A CN201610896614.1A CN201610896614A CN106345494A CN 106345494 A CN106345494 A CN 106345494A CN 201610896614 A CN201610896614 A CN 201610896614A CN 106345494 A CN106345494 A CN 106345494A
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- visible light
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- degradation agent
- deionized water
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- 230000015556 catabolic process Effects 0.000 title claims abstract description 45
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002135 nanosheet Substances 0.000 title claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 229910001449 indium ion Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 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
- 238000005406 washing Methods 0.000 claims abstract description 8
- -1 sulfur ions Chemical class 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- 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
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 238000012805 post-processing Methods 0.000 claims description 2
- 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 15
- 229940043267 rhodamine b Drugs 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 10
- 229910052717 sulfur Inorganic materials 0.000 abstract description 6
- 239000011593 sulfur Substances 0.000 abstract description 6
- 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 5
- 229940012189 methyl orange Drugs 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000007935 neutral effect Effects 0.000 abstract 1
- 229940069002 potassium dichromate Drugs 0.000 abstract 1
- 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 1
- 238000003828 vacuum filtration Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 13
- 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 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 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
- 230000003287 optical effect Effects 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000012360 testing method 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
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 229950000845 politef Drugs 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
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 238000012827 research and development Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 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
- 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
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 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
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 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
- 230000005611 electricity Effects 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
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000011160 research Methods 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
- 230000001629 suppression Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 238000005303 weighing 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—
-
- B01J35/39—
-
- 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
Abstract
The invention relates to a preparation method of a high-efficiency visible light degradation agent nanosheet In2.77S4. The method comprises the following steps: A. material preparation: sufficiently dissolving In(NO3)3.4.5H2O and thioacetamide in deionized water, and putting the sollution in a teflon-lined hydrothermal reaction kettle, wherein the indium ion concentration is 0.05 mol/L, and the mole ratio of indium ions to sulfur ions is 1:3-1:5; B. reaction: reacting for 14-16 hours while controlling the hydrothermal reaction temperature at 180 DEG C, and after the reaction finishes, naturally cooling the reaction kettle to room temperature; and C. after-treatment: taking the product out of the reaction kettle, repeatedly washing with deionized water, carrying out vacuum filtration to a neutral state, and drying to obtain the sheet In2.77S4. The method has the advantages of simple technique, mild reaction conditions, short technical process and high preparation efficiency. The obtained product has high degradation efficiency for rhodamine B, methyl orange and potassium dichromate under visible light.
Description
Technical field
The invention belongs to photodegradable aid field of material technology, it is 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 the Organic substance in water body and heavy metal is always the great difficult problem perplexing the mankind, the birth of photodegradable aid
The raw dawn providing " green, environmental protection " for solving this difficult problem, but traditional photodegradable aid such as tio2, zno etc., energy gap
More than 2.9ev, greater band gap, insensitive to visible ray and infrared light, only there is preferable degradation effect under ultraviolet light, and purple
Outer light accounting in whole sunlight is only 5% about.Therefore, the disposal efficiency, the efficiency light fall obtaining under visible ray are improved
Solution agent becomes world's focus in recent years.It is generally acknowledged that: the material that energy gap is less than 2.9ev has preferably under visible light
Response range.Based on this, energy gap becomes an important indicator weighing photodegradable aid photoresponse degree.Metal vulcanizes
The energy gap of thing is less than 2.9ev mostly, and many scholars have made substantial amounts of research to this series compound, obtain a series of can
The achievement of happiness, has significantly promoted the development in light degradation field.For example: luo et al. is with sncl4·5h2O is raw material with thiourea, uses water
Full-boiled process has synthesized lamella sns2, the energy gap of this material is 2.1ev, the methyl orange of 60min degradable 35%；Yang et al. with
zncl2、incl3·4h2O, thioacetamide are raw material, the lamella znin with solvent structure2s4, the energy gap of this 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, has synthesized petal-shaped in hydro-thermal method2s3, the energy gap of this material is 2.0ev, 60min degradable 90%
2,4- chlorophenesic acid；It should be noted that: Wang et al. is in cn102335616 with incl3·4h2O and thioacetamide are former
Material, has synthesized the in of bouquet shape with hydro-thermal method2s3, the methyl orange of the degradable in 2.5h 90% of this material, there is preferable reality
Use effect.But, the synthetic method of above-mentioned degradation agent is more complicated, and technological process is long, and preparation efficiency is low.And how existing
In technical foundation, research and development one kind can improve degradation effect further, and method is simple, and technological process is short, and what preparation efficiency was high can
See that photodegradable aid material is the target of our research and development.
Content of the invention
The present invention is to comply with above-mentioned R＆D target, devises a kind of efficient visible light degradation agent nano-sheet in2.77s4System
Preparation Method, the method is simple, reaction condition is gentle, technological process is short, preparation efficiency is high and the energy gap of the product of synthesis is little,
There is excellent photoresponse effect under visible light.
The technical solution used in the present invention is, a kind of efficient visible light degradation agent nano-sheet in2.77s4Preparation method,
Comprise the following steps:
A, get the raw materials ready:
Indium nitrate hydrate, thioacetamide is taken to be completely dissolved in deionized water, wherein, indium ion concentration is
The mol ratio of 0.05mol/l, indium ion and sulphion is 1:3-1:5, is placed in the hydro-thermal reaction of inner liner polytetrafluoroethylene afterwards
In kettle；
B, reaction:
Hydrothermal temperature is controlled to be 180 DEG C, the response time is 14-16 hour, and it is naturally cold that question response terminates rear reactor
But to room temperature；
C, post processing:
Product in reactor is taken out, is dried after deionized water cyclic washing, sucking filtration to neutrality, to obtain lamellar
in2.77s4.
Described indium nitrate hydrate is in (no3)3·4.5h2o.
Lamellar in of step c gained2.77s4Thickness be 5-20nm.
Preferably, lamellar in of step c gained2.77s4Thickness be 10nm.
The invention has the beneficial effects as follows: adjustment raw material, indium nitrate hydrate, thioacetamide are completely dissolved in deionization
In water, control the mol ratio of indium ion and sulphion, be placed in afterwards in the hydrothermal reaction kettle of inner liner polytetrafluoroethylene, by control
Response time processed and temperature, a step Fast back-projection algorithm goes out efficient visible light degradation agent nano-sheet in2.77s4, the forbidden band width of this product
Degree is little, has excellent photoresponse effect under visible light, be reported at present the material best to rhodamine b degradation effect it
One, this product is high to methyl orange and potassium dichromate degradation efficiency simultaneously, to the dirt solving Organic substance and heavy metal in water pollution
Dye problem has significant reference and wide application prospect.
Brief description
Fig. 1 is the transmission electron microscope figure of product in embodiment 2.
Fig. 2 is the X-ray diffraction pattern of product in embodiment 2.
Fig. 3 be embodiment 2 in product ultraviolet-diffuse spectrogram.
Fig. 4 is product degradation effect figure under visible light in embodiment 2.
Fig. 5 is the degradation effect figure that in embodiment 2, product adds different sacrifice agents under visible light.
Specific embodiment
With specific embodiment, invention is described further below in conjunction with the accompanying drawings:
Embodiment 1
1st, weigh appropriate in (no3)3·4.5h2O (Chemical Reagent Co., Ltd., Sinopharm Group, similarly hereinafter), thioacetamide
(Chemical Reagent Co., Ltd., Sinopharm Group, similarly hereinafter) is completely dissolved in deionized water, is placed in inner liner polytetrafluoroethylene afterwards
In hydrothermal reaction kettle；Wherein, the mol ratio for 0.05mol/l, indium and sulfur for the indium ion concentration is 1:3.
2nd, hydrothermal temperature is controlled to be 180 DEG C, the response time is 14h, reaction terminates rear reactor and naturally cools to room
Temperature.
3rd, the product in step 2 is taken out from reactor, be dried after deionized water cyclic washing sucking filtration to neutrality, obtain
To the powder in for 5nm for the lamellar spacing2.77s4.
4th, weigh the in of 0.05g2.77s4Product, be respectively placed in 10mg/l rhodamine b solution, the methyl orange solution of 10mg/l,
In the potassium bichromate solution of 70mg/l, carry out photocatalytic degradation experiment under the xenon lamp irradiation of 300w, adopted in illumination
Optical filter filters off ultraviolet light.Test result indicate that, the in obtaining under the conditions of being somebody's turn to do2.77s4To rhodamine b solution degradation rate in 9min
Reach 98%, in 30min, the degradation rate of methyl orange solution is reached with 87%, in 60min, the degradation rate of potassium bichromate solution is reached
86%.
Embodiment 2
1st, weigh appropriate in (no3)3·4.5h2O, thioacetamide are completely dissolved in deionized water, are placed in liner afterwards
In the hydrothermal reaction kettle of politef；Wherein, the mol ratio for 0.05mol/l, indium and sulfur for the indium ion concentration is 1:4.
2nd, hydrothermal temperature is controlled to be 180 DEG C, the response time is 15h, reaction terminates rear reactor and naturally cools to room
Temperature.
3rd, the product in step 2 is taken out from reactor, is dried after deionized water cyclic washing, sucking filtration to neutrality,
Obtain the powder in that lamellar spacing is 10nm2.77s4.
4th, weigh the in of 0.05g2.77s4Product, be respectively placed in 10mg/l rhodamine b solution, the methyl orange solution of 10mg/l,
In the potassium bichromate solution of 70mg/l, carry out photocatalytic degradation experiment under the xenon lamp irradiation of 300w, adopted in illumination
Optical filter filters off ultraviolet light.Test result indicate that, the in obtaining under the conditions of being somebody's turn to do2.77s4To rhodamine b solution degradation rate in 9min
Reach 99.9%, in 30min, the degradation rate of methyl orange solution is reached with 88%, in 60min, the degradation rate of potassium bichromate solution is reached
87%.
The transmission electron microscope figure for product of Fig. 1 description, as can be seen from Figure, the pattern of products obtained therefrom is tied for lamellar
Structure, the thickness of lamella is 10nm；The X-ray diffraction pattern for product of Fig. 2 description, knowable to figure, the characteristic diffraction peak 2 of this 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) consistent, the indices of crystallographic plane correspond respectively to (220), (311), (222), (400),
(511)、(440)、(533)、(444)、(800)；Fig. 3 description the ultraviolet for product-diffuse spectrogram, can from figure
Go out, in2.77s4Wider to the response range of visible ray, to visible light-responded substantially, energy gap is 1.75ev hence it is evident that being less than
2.9ev, is one of currently reported minimum energy gap；The degradation effect figure under visible light for product of Fig. 4 description,
As can be seen from Figure, in2.77s4In 9min, 99.9% is reached to rhodamine b solution degradation rate, in 30min to methyl orange solution
Degradation rate reaches 88%, in 60min, the degradation rate of potassium bichromate solution is reached with 87%, fully shows this product and has excellent fall
Solution effect, and to gas chromatography/heavy metal, there is effect simultaneously.Fig. 5 is that in embodiment 2, product adds difference under visible light
The degradation effect figure of sacrifice agent, this figure can reflect the light degradation mechanism of product, and concrete operations are as follows: weigh 0.05g in2.77s4
Product, is placed in 10mg/l rhodamine b solution, adds sacrifice agent before adding light source, and later step is identical with step 4, sacrificial
Domestic animal agent is ethylenediaminetetraacetic acid or sodium bicarbonate.Experimental result shows, the light degradation before and after contrast adds ethylenediaminetetraacetic acid is imitated
Really, product is changed into 90% to the degradation rate of rhodamine b solution from 99.9% in 9min, and this explanation ethylenediaminetetraacetic acid drops to light
Solution suppression is simultaneously inconspicuous, that is, hole is less to photodegradative effect；And after adding sodium bicarbonate, product is in 9min to Luo Dan
The degradation rate of bright b solution is changed into 30% from 99.9%, and this explanation sodium bicarbonate has significantly inhibitory action, Yi Ji electricity to light degradation
Son plays a leading role during photodegradative.
Embodiment 3
1st, weigh appropriate in (no3)3·4.5h2O, thioacetamide are completely dissolved in deionized water, are placed in liner afterwards
In the hydrothermal reaction kettle of politef；Wherein, the mol ratio for 0.05mol/l, indium and sulfur for the indium ion concentration is 1:5.
2nd, hydrothermal temperature is controlled to be 180 DEG C, the response time is 14h, reaction terminates rear reactor and naturally cools to room
Temperature.
3rd, the product in step 2 is taken out from reactor, be dried after deionized water cyclic washing sucking filtration to neutrality, obtain
To the powder in for 20nm for the lamellar spacing2.77s4.
4th, weigh the in of 0.05g2.77s4Product, be respectively placed in 10mg/l rhodamine b solution, the methyl orange solution of 10mg/l,
In the potassium bichromate solution of 70mg/l, carry out photocatalytic degradation experiment under the xenon lamp irradiation of 300w, adopted in illumination
Optical filter filters off ultraviolet light.Test result indicate that, the in obtaining under the conditions of being somebody's turn to do2.77s4To rhodamine b solution degradation rate in 9min
Reach 93%, in 30min, the degradation rate of methyl orange solution is reached with 85%, in 60min, the degradation rate of potassium bichromate solution is reached
86%.
Example 4:
1st, weigh appropriate in (no3)3·4.5h2O, thioacetamide are completely dissolved in deionized water, are placed in liner afterwards
In the hydrothermal reaction kettle of politef；Wherein, the mol ratio for 0.05mol/l, indium and sulfur for the indium ion concentration is 1:3.
2nd, hydrothermal temperature is controlled to be 180 DEG C, the response time is 16h, reaction terminates rear reactor and naturally cools to room
Temperature.
3rd, the product in step 2 is taken out from reactor, be dried after deionized water cyclic washing sucking filtration to neutrality, obtain
To the powder in for 16nm for the lamellar spacing2.77s4.
4th, weigh the in of 0.05g2.77s4Product, be respectively placed in 10mg/l rhodamine b solution, the methyl orange solution of 10mg/l,
In the potassium bichromate solution of 70mg/l, carry out photocatalytic degradation experiment under the xenon lamp irradiation of 300w, adopted in illumination
Optical filter filters off ultraviolet light.Test result indicate that, the in obtaining under the conditions of being somebody's turn to do2.77s4To rhodamine b solution degradation rate in 9min
Reach 94%, in 30min, the degradation rate of methyl orange solution is reached with 83%, in 60min, the degradation rate of potassium bichromate solution is reached
84%.
Example 5:
1st, weigh appropriate in (no3)3·4.5h2O, thioacetamide are completely dissolved in deionized water, are placed in liner afterwards
In the hydrothermal reaction kettle of politef；Wherein, the mol ratio for 0.05mol/l, indium and sulfur for the indium ion concentration is 1:4.
2nd, hydrothermal temperature is controlled to be 180 DEG C, the response time is 16h, reaction terminates rear reactor and naturally cools to room
Temperature.
3rd, the product in step 2 is taken out from reactor, be dried after deionized water cyclic washing sucking filtration to neutrality, obtain
To the powder in for 7nm for the lamellar spacing2.77s4.
4th, weigh the in of 0.05g2.77s4Product, be respectively placed in 10mg/l rhodamine b solution, the methyl orange solution of 10mg/l,
In the potassium bichromate solution of 70mg/l, carry out photocatalytic degradation experiment under the xenon lamp irradiation of 300w, adopted in illumination
Optical filter filters off ultraviolet light.Test result indicate that, the in obtaining under the conditions of being somebody's turn to do2.77s4To rhodamine b solution degradation rate in 9min
Reach 98%, in 30min, the degradation rate of methyl orange solution is reached with 88%, in 60min, the degradation rate of potassium bichromate solution is reached
87%.
Claims (4)
1. a kind of efficient visible light degradation agent nano-sheet in2.77s4Preparation method it is characterised in that: described method and step
Include:
A, get the raw materials ready:
Take indium nitrate hydrate, thioacetamide to be completely dissolved in deionized water, wherein, indium ion concentration be 0.05mol/l,
The mol ratio of indium ion and sulphion is 1:3-1:5, is placed in afterwards in the hydrothermal reaction kettle of inner liner polytetrafluoroethylene；
B, reaction:
Hydrothermal temperature is controlled to be 180 DEG C, the response time is 14-16 hour, question response terminates rear reactor and naturally cools to
Room temperature；
C, post processing:
Product in reactor is taken out, is dried after deionized water cyclic washing, sucking filtration to neutrality, to obtain lamellar
in2.77s4.
2. a kind of efficient visible light degradation agent nano-sheet according to claim 12.77s4Preparation method, its feature
It is: described 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, its feature
It is: lamellar in of step c gained2.77s4Thickness be 5-20nm.
4. a kind of efficient visible light degradation agent nano-sheet according to claim 32.77s4Preparation method, its feature
It is: lamellar in of step c gained2.77s4Thickness be 10nm.
Priority Applications (1)
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| CN107841791A (en) * | 2017-11-07 | 2018-03-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of monocrystalline indium nano wire and products thereof and application |
| CN115959701A (en) * | 2023-02-20 | 2023-04-14 | 西南交通大学 | Preparation method and application of 3D self-assembly hydrangea-shaped indium sulfide |
| CN115959701B (en) * | 2023-02-20 | 2024-04-26 | 西南交通大学 | Preparation method and application of 3D self-assembled hydrangea-shaped indium sulfide |
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Cited By (4)
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| CN107841791A (en) * | 2017-11-07 | 2018-03-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of monocrystalline indium nano wire and products thereof and application |
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| CN115959701A (en) * | 2023-02-20 | 2023-04-14 | 西南交通大学 | Preparation method and application of 3D self-assembly hydrangea-shaped indium sulfide |
| CN115959701B (en) * | 2023-02-20 | 2024-04-26 | 西南交通大学 | Preparation method and application of 3D self-assembled hydrangea-shaped indium sulfide |
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