CN104607170A - Heterostructure material In2O3/In2TiO5, as well as application and preparation method thereof - Google Patents
Heterostructure material In2O3/In2TiO5, as well as application and preparation method thereof Download PDFInfo
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- CN104607170A CN104607170A CN201510004887.6A CN201510004887A CN104607170A CN 104607170 A CN104607170 A CN 104607170A CN 201510004887 A CN201510004887 A CN 201510004887A CN 104607170 A CN104607170 A CN 104607170A
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Abstract
The invention discloses a heterostructure material In2O3/In2TiO5, as well as application and a preparation method thereof. The heterostructure material In2O3/In2TiO5 comprises In2O3 and In2TiO5, and is prepared by the following steps: using glycine, indium nitrate, butyl titanate and nitrocellulose as raw materials, wherein the ratio of indium nitrate to butyl titanate is 2 to 1, and performing high-temperature roasting. The heterostructure material In2O3/In2TiO5 is prepared for the first time, is used as a photocatalytic material, is mild in synthesis condition, stable in performance, and high in activity, can be repeatedly used, can be used for photolysis and purification of toxic and harmful chemical substances such as antibiotics or dyes in wastewater in UV-light and visible light, solves the technical problem that a traditional photocatalyst cannot realize photolysis and purification of toxic and harmful chemical substances such as antibiotics or dyes in wastewater in visible light, and enriches the varieties of photocatalysts.
Description
Technical field
The invention belongs to technical field of material, be specifically related to a kind of heterogeneous structure material In
2o
3/ In
2tiO
5, also relate to above-mentioned heterogeneous structure material In
2o
3/ In
2tiO
5application and preparation method.
Background technology
Along with the continuous quickening of process of industrialization and the expansion of human lives's scope, water pollution problem is day by day serious, and the discharge of a large amount of waste water makes people's lives environmental quality go from bad to worse.Wherein, antibiotic waste water, owing to being difficult to containing bio-toxicity material realize traditional raw degraded, becomes a great problem of water treatment field.As the photocatalysis method of one of high-level oxidation technology, be widely used in the application study of Degradation of Antibiotics.Titanate nano material has higher mechanical performance, excellent physical property, preferably heat endurance and chemical stability, excellent electric property and optical property, is developed rapidly in fields such as electricity, magnetics, pottery and photocatalysis.Wherein, In
2tiO
5structure cell be by [InO
6] and [TiO
6] octahedron composition, have three-dimensional tunnel structure, the octahedral structure in crystal is conducive to the transfer of electron stream, and it is n-type semiconductor, only has response to ultraviolet light, does not have photocatalytic activity at radiation of visible light.
Summary of the invention
A kind of heterogeneous structure material In that the object of this invention is to provide
2o
3/ In
2tiO
5, solve the photochemical catalyst that exists in prior art cannot in visible-range the technical problem of catalysis light degradation toxicant.
The second object of the present invention is to provide above-mentioned heterogeneous structure material In
2o
3/ In
2tiO
5application.
The third object of the present invention is to provide above-mentioned heterogeneous structure material In
2o
3/ In
2tiO
5preparation method.
The fourth object of the present invention is to provide the heterogeneous structure material In prepared by above-mentioned preparation method
2o
3/ In
2tiO
5application.
The first technical scheme that the present invention adopts is, a kind of heterogeneous structure material In
2o
3/ In
2tiO
5, by In
2o
3and In
2tiO
5form, top layer is In
2o
3, internal layer is In
2tiO
5.
The second technical scheme that the present invention adopts is, above-mentioned heterogeneous structure material In
2o
3/ In
2tiO
5application, it is used as the photochemical catalyst of ultraviolet light or Visible Light Induced Photocatalytic rhodamine B, methylene blue, lavo-ofloxacin.
The 3rd technical scheme that the present invention adopts is, above-mentioned heterogeneous structure material In
2o
3/ In
2tiO
5preparation method, implement according to following steps:
Step 1: ethylene glycol solution glycine solid being configured to 0.2wt% ~ 0.5wt%, after heating water bath magnetic agitation, obtains clear transparent solutions a;
Step 2: by the In (NO of 2/3 glycine amount of substance
3)
34.5H
2o is dissolved in ethylene glycol, is made into the In (NO that concentration is 0.1mol/L
3)
3ethylene glycol solution, dropped in solution a, then after heating water bath magnetic agitation, obtained solution b;
Step 3: drop in solution b by the butyl titanate of 1/3 glycine amount of substance, then after heating water bath magnetic agitation, obtains yellow solution c;
Step 4: the nitrocellulose accounting for yellow solution c quality 0.15% ~ 0.2% is added in solution c, ultrasonic 30 ~ 60min, obtains suspension d;
Step 5: evaporated in 130 ~ 140 DEG C of oil baths by the suspension d obtained in step 4, until suspension d becomes white solid, stops heating;
Step 6: by white solid on 80 ~ 100 DEG C of heating plates, make nitrocellulose primary combustion, obtain black solid e;
Step 7: foam black solid e at 150 ~ 190 DEG C 10 ~ 30min, obtains dark gray powder, and by powder transfer in ceramic crucible;
Step 8: ceramic crucible is placed in Muffle furnace, is warming up to 200 ~ 300 DEG C with 5 DEG C/min, constant temperature 30 ~ 60min, be warming up to 400 ~ 500 DEG C with 2 DEG C/min again, constant temperature 30 ~ 60min, be finally warming up to 800 DEG C with 10 DEG C/min, constant temperature 2h, naturally cools to room temperature, obtains heterogeneous structure material In
2o
3/ In
2tiO
5.
The feature of the 3rd technical scheme that the present invention adopts also is,
In step 1, the temperature of heating water bath is 75 ~ 85 DEG C, and the time of magnetic agitation is 30 ~ 60min.
In (NO in step 2
3)
3ethylene glycol solution concentration be 0.1 ~ 0.3mol/L, rate of addition is 20 ~ 30/min, and the temperature of heating water bath is 75 ~ 85 DEG C, and the time of magnetic agitation is 30 ~ 60min.
In step 3, the rate of addition of butyl titanate is 20 ~ 30/min, and the temperature of heating water bath is 75 ~ 85 DEG C, and the time of magnetic agitation is 90 ~ 150min.
The 4th technical scheme that the present invention adopts is, the heterogeneous structure material In prepared by above-mentioned preparation method
2o
3/ In
2tiO
5application, it is used as the photochemical catalyst of ultraviolet light or Visible Light Induced Photocatalytic rhodamine B, methylene blue, lavo-ofloxacin.
The invention has the beneficial effects as follows, the present invention prepares heterogeneous structure material In first
2o
3/ In
2tiO
5, and use it for photocatalysis field.The present invention prepares In
2o
3/ In
2tiO
5synthesis condition gentle, stable performance, active high, reusable, it all can the toxic and harmful substance such as antibiotic or dyestuff in light decomposing, purifying process waste water under ultraviolet light and visible ray, overcoming traditional photochemical catalyst can not the technical problem of the toxic and harmful substance such as antibiotic or dyestuff in visible-range in light decomposing, purifying process waste water, has enriched the kind of photochemical catalyst.
Accompanying drawing explanation
Fig. 1 is heterojunction structure photochemical catalyst In prepared by the inventive method
2o
3/ In
2tiO
5xRD figure;
Fig. 2 is heterojunction structure photochemical catalyst In prepared by the inventive method
2o
3/ In
2tiO
5sEM photo under different amplification;
Fig. 3 is absorbance change curve (a) figure of photocatalyst for degrading rhodamine B prepared by the present invention is the absorbance change curve under 125W Hg lamp irradiation, and (b) figure is the absorbance change curve under 150W xenon lamp irradiates; Experiment condition is: reactant liquor is the rhodamine B solution 50mL of 10mg/L, and the addition of photochemical catalyst is 0.1g.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
One of the present invention prepares heterogeneous structure material In
2o
3/ In
2tiO
5method, specifically carry out according to following steps:
Step 1: ethylene glycol solution glycine solid being configured to 0.2wt% ~ 0.5wt%, 75 ~ 85 DEG C of water-bath magnetic agitation 30 ~ 60min, obtain clear transparent solutions a;
Step 2: by the In (NO of 2/3 glycine amount of substance
3)
34.5H
2o is dissolved in ethylene glycol, is made into the In (NO that concentration is 0.1mol/L
3)
3ethylene glycol solution, it is slowly dropped in solution a with the speed of 20 ~ 30/min, then under 75 ~ 85 DEG C of water-baths in magnetic agitation 30 ~ 60min, obtain solution b;
Step 3: the butyl titanate of 1/3 glycine amount of substance is slowly dropped in solution b with the speed of 20 ~ 30/min, magnetic agitation 90 ~ 150min in then under 75 ~ 85 DEG C of water-baths, stops heating water bath, obtains yellow solution c;
Step 4: the nitrocellulose accounting for yellow solution c quality 0.15% ~ 0.2% is added in solution c, ultrasonic 30 ~ 60min, obtains suspension d;
Step 5: evaporated in 130 ~ 140 DEG C of oil baths by the suspension d obtained in step 4, until suspension d becomes white solid, stops heating;
Step 6: by white solid on the heating plate of 80 ~ 100 DEG C, make nitrocellulose primary combustion, obtain black solid e;
Step 7: foam black solid e at 150 ~ 190 DEG C 10 ~ 30min, obtains dark gray powder, and by powder transfer in ceramic crucible;
Step 8: ceramic crucible is placed in Muffle furnace, 200 ~ 300 DEG C are warming up to 5 DEG C/min, constant temperature 30 ~ 60min, 400 ~ 500 DEG C are warming up to again with 2 DEG C/min, constant temperature 30 ~ 60min, is finally warming up to 800 DEG C with 10 DEG C/min, constant temperature 2h, naturally cool to room temperature, obtain heterojunction structure catalysis material In
2o
3/ In
2tiO
5.
Known see Fig. 1, be that In appears in the places such as 13.58 °, 17.06 °, 27.36 °, 30.55 °, 31.23 °, 35.63 °, 36.16 °, 41.68 °, 51.68 °, 51.80 °, 52.19 °, 60.46 °, 61.57 °, 61.69 ° and 61.98 ° at 2 θ
2tiO
5the characteristic diffraction peak of (JCPDS No.82-0326), being 21.44 °, 30.51 °, 50.89 ° and 60.51 ° at 2 θ there is In simultaneously
2o
3the characteristic peak of (JCPDS No.65-3170), this illustrates that this photochemical catalyst is by In
2tiO
5and In
2o
3be composited.
Known see Fig. 2, In prepared by the present invention
2tiO
5/ In
2o
3for cappelletti bag-like mesoporous material, top layer is In
2o
3, internal layer is In
2tiO
5, and top layer and internal layer all have certain mesoporous, and be not In
2o
3and In
2tiO
5simple mixing.
Known see Fig. 3, under mercury lamp and xenon lamp irradiation, along with the prolongation of light application time, the absorbance of rhodamine B solution reduces gradually, and there is certain blue-shifted phenomenon (second class process is gone in the degradation process existence of rhodamine B), show that rhodamine B solution is degraded under the irradiation of mercury lamp, xenon lamp, as calculated, after mercury lamp, xenon lamp irradiation 180min, the clearance difference 92.1%, 71.2% of rhodamine B.This shows, this photochemical catalyst not only shows excellent catalytic activity under ultraviolet light, shows certain visible light catalysis activity simultaneously.
The present invention prepares heterogeneous structure material In first
2o
3/ In
2tiO
5, and use it for photocatalysis field.The present invention prepares In
2o
3/ In
2tiO
5synthesis condition gentle, stable performance, active high, reusable, it all can the toxic and harmful substance such as antibiotic or dyestuff in light decomposing, purifying process waste water under ultraviolet light and visible ray, overcoming traditional photochemical catalyst can not the technical problem of the toxic and harmful substance such as antibiotic or dyestuff in visible-range in light decomposing, purifying process waste water, has enriched the kind of photochemical catalyst.
Embodiment 1
0.1125g glycine solid is mixed with the ethylene glycol solution of the glycine of 0.2wt%, 80 DEG C of water bath with thermostatic control lower magnetic forces stir 30min, obtain clear transparent solutions a; By the In (NO of 0.3818g
3)
34.5H
2o is dissolved in ethylene glycol, is made into the In (NO that concentration is 0.1mol/L
3)
3ethylene glycol solution, slowly drop in solution a with the speed of 20/min, then under 75 DEG C of waters bath with thermostatic control in magnetic agitation 30min, obtain solution b; 0.17g butyl titanate is slowly dropped in solution b with the speed of 20/min, then magnetic agitation 120min in 75 DEG C of waters bath with thermostatic control, stop heating water bath, obtain yellow solution c; The nitrocellulose accounting for yellow solution c quality 0.15% is added in solution c, ultrasonic 30min, obtains suspension d; Suspension d is evaporated in 130 DEG C of oil baths, until suspension d becomes white solid, stops heating, then white solid is placed on 80 DEG C of constant temperature heating plates, make nitrocellulose primary combustion, obtain black solid e; Then foam black solid e at 190 DEG C 20min, obtains dark gray powder, and by powder transfer in ceramic crucible; Finally ceramic crucible is placed in Muffle furnace, is warming up to 250 DEG C with 5 DEG C/min, constant temperature 60min, then be warming up to 500 DEG C with 2 DEG C/min, constant temperature 45min, be finally warming up to 800 DEG C with 10 DEG C/min, constant temperature 2h, naturally cools to room temperature, obtains heterogeneous structure material In
2o
3/ In
2tiO
5.
Embodiment 2
0.55g glycine solid is mixed with the ethylene glycol solution of the glycine of 0.4wt%, 75 DEG C of water bath with thermostatic control lower magnetic forces stir 40min, obtain clear transparent solutions a; By the In (NO of 1.8666g
3)
34.5H
2o is dissolved in ethylene glycol, is made into the In (NO that concentration is 0.2mol/L
3)
3ethylene glycol solution, slowly drop in solution a with the speed of 30/min, then under 85 DEG C of waters bath with thermostatic control in magnetic agitation 40min, obtain solution b; The butyl titanate of 0.8311g is slowly dropped in solution b with the speed of 25/min, then magnetic agitation 90min in 85 DEG C of waters bath with thermostatic control, stop heating water bath, obtain yellow solution c; The nitrocellulose accounting for yellow solution c quality 0.2% is added in solution c, ultrasonic 45min, obtains suspension d; Suspension d is evaporated in 140 DEG C of oil baths, until suspension d becomes white solid, stops heating, then white solid is placed on 90 DEG C of constant temperature heating plates, make nitrocellulose primary combustion, obtain black solid e; Then foam black solid e at 150 DEG C 30min, obtains dark gray powder, and by powder transfer in ceramic crucible; Finally ceramic crucible is placed in Muffle furnace, is warming up to 200 DEG C with 5 DEG C/min, constant temperature 30min, then be warming up to 400 DEG C with 2 DEG C/min, constant temperature 30min, be finally warming up to 800 DEG C with 10 DEG C/min, constant temperature 2h, naturally cools to room temperature, obtains heterogeneous structure material In
2o
3/ In
2tiO
5.
Embodiment 3
1.3g glycine solid is mixed with the ethylene glycol solution of the glycine of 0.5wt%, 85 DEG C of water bath with thermostatic control lower magnetic forces stir 60min, obtain clear transparent solutions a; By the In (NO of 4.4119g
3)
34.5H
2o is dissolved in ethylene glycol, is made into the In (NO that concentration is 0.3mol/L
3)
3ethylene glycol solution, slowly drop in solution a with the speed of 25/min, then under 80 DEG C of waters bath with thermostatic control in magnetic agitation 60min, obtain solution b; The butyl titanate of 1.9644g is slowly dropped in solution b with the speed of 30/min, then magnetic agitation 150min in 80 DEG C of waters bath with thermostatic control, stop heating water bath, obtain yellow solution c; The nitrocellulose accounting for yellow solution c quality 0.18% is added in solution c, ultrasonic 60min, obtains suspension d; Suspension d is evaporated in 135 DEG C of oil baths, until suspension d becomes white solid, stops heating, then white solid is placed on 100 DEG C of constant temperature heating plates, make nitrocellulose primary combustion, obtain black solid e; Then foam black solid e at 180 DEG C 10min, obtains dark gray powder, and by powder transfer in ceramic crucible; Finally ceramic crucible is placed in Muffle furnace and is warming up to 300 DEG C with 5 DEG C/min, constant temperature 40min, then be warming up to 450 DEG C with 2 DEG C/min, constant temperature 60min, constant temperature 2h after being finally warming up to 800 DEG C with 10 DEG C/min, naturally cools to room temperature, obtains heterogeneous structure material In
2o
3/ In
2tiO
5.
Claims (7)
1. a heterogeneous structure material In
2o
3/ In
2tiO
5, it is characterized in that, described heterogeneous structure material is by In
2o
3and In
2tiO
5form, top layer is In
2o
3, internal layer is In
2tiO
5.
2. a kind of heterogeneous structure material according to claim 1
2o
3/ In
2tiO
5application, it is characterized in that, it is used as the photochemical catalyst of ultraviolet light or Visible Light Induced Photocatalytic rhodamine B, methylene blue, lavo-ofloxacin.
3. a kind of heterogeneous structure material according to claim 1
2o
3/ In
2tiO
5preparation method, it is characterized in that, implement according to following steps:
Step 1: ethylene glycol solution glycine solid being configured to 0.2wt% ~ 0.5wt%, after heating water bath magnetic agitation, obtains clear transparent solutions a;
Step 2: by the In (NO of 2/3 glycine amount of substance
3)
34.5H
2o is dissolved in ethylene glycol, obtains In (NO
3)
3ethylene glycol solution, dropped in solution a, then after heating water bath magnetic agitation, obtained solution b;
Step 3: drop in solution b by the butyl titanate of 1/3 glycine amount of substance, then after heating water bath magnetic agitation, obtains yellow solution c;
Step 4: the nitrocellulose accounting for yellow solution c quality 0.15% ~ 0.2% is added in solution c, ultrasonic 30 ~ 60min, obtains suspension d;
Step 5: evaporated in 130 ~ 140 DEG C of oil baths by the suspension d obtained in step 4, until suspension d becomes white solid, stops heating;
Step 6: by white solid on 80 ~ 100 DEG C of heating plates, make nitrocellulose primary combustion, obtain black solid e;
Step 7: foam black solid e at 150 ~ 190 DEG C 10 ~ 30 min, obtains dark gray powder, and by powder transfer in ceramic crucible;
Step 8: ceramic crucible is placed in Muffle furnace, is warming up to 200 ~ 300 DEG C with 5 DEG C/min, constant temperature 30 ~ 60min, be warming up to 400 ~ 500 DEG C with 2 DEG C/min again, constant temperature 30 ~ 60min, be finally warming up to 800 DEG C with 10 DEG C/min, constant temperature 2h, naturally cools to room temperature, obtains heterogeneous structure material In
2o
3/ In
2tiO
5.
4. a kind of heterogeneous structure material according to claim 3
2o
3/ In
2tiO
5preparation method, it is characterized in that, in step 1, the temperature of heating water bath is 75 ~ 85 DEG C, and the time of magnetic agitation is 30 ~ 60min.
5. a kind of heterogeneous structure material according to claim 3
2o
3/ In
2tiO
5preparation method, it is characterized in that, In (NO in step 2
3)
3ethylene glycol solution concentration be 0.1 ~ 0.3mol/L, rate of addition is 20 ~ 30/min, and the temperature of heating water bath is 75 ~ 85 DEG C, and the time of magnetic agitation is 30 ~ 60min.
6. a kind of heterogeneous structure material according to claim 3
2o
3/ In
2tiO
5preparation method, it is characterized in that, in step 3, the rate of addition of butyl titanate is 20 ~ 30/min, and the temperature of heating water bath is 75 ~ 85 DEG C, and the time of magnetic agitation is 90 ~ 150min.
7. a kind of heterogeneous structure material according to any one of claim 3 to 6
2o
3/ In
2tiO
5the In for preparing of preparation method
2o
3/ In
2tiO
5application, it is characterized in that, it is used as the photochemical catalyst of ultraviolet light or Visible Light Induced Photocatalytic rhodamine B, methylene blue, lavo-ofloxacin.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510004887.6A CN104607170B (en) | 2015-01-06 | 2015-01-06 | Heterostructure material In2O3/In2TiO5, as well as application and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510004887.6A CN104607170B (en) | 2015-01-06 | 2015-01-06 | Heterostructure material In2O3/In2TiO5, as well as application and preparation method thereof |
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|---|---|
| CN104607170A true CN104607170A (en) | 2015-05-13 |
| CN104607170B CN104607170B (en) | 2017-01-18 |
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|---|---|---|---|
| CN201510004887.6A Expired - Fee Related CN104607170B (en) | 2015-01-06 | 2015-01-06 | Heterostructure material In2O3/In2TiO5, as well as application and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106356291A (en) * | 2016-09-14 | 2017-01-25 | 齐鲁工业大学 | Low temperature solution method for preparing indium-titanium-oxide transparent semiconductor film |
| CN110038594A (en) * | 2019-05-13 | 2019-07-23 | 东北师范大学 | A kind of preparation method of porous oxidation indium/indium sulfide heterojunction material |
| CN115634685A (en) * | 2022-11-03 | 2023-01-24 | 常熟理工学院 | Photocatalytic material responding to visible light and preparation method thereof |
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| JP2013154296A (en) * | 2012-01-30 | 2013-08-15 | Kubota Corp | Water treatment filter medium, and purification tank |
| CN103706350A (en) * | 2014-01-06 | 2014-04-09 | 齐鲁工业大学 | In2O3/ZnO heterostructure nanotube as well as preparation method and application thereof |
| CN103877969A (en) * | 2014-04-08 | 2014-06-25 | 中南大学 | In 2 O 3 ·InVO 4 Heterostructure composites and methods of making and using same |
-
2015
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2013154296A (en) * | 2012-01-30 | 2013-08-15 | Kubota Corp | Water treatment filter medium, and purification tank |
| CN103706350A (en) * | 2014-01-06 | 2014-04-09 | 齐鲁工业大学 | In2O3/ZnO heterostructure nanotube as well as preparation method and application thereof |
| CN103877969A (en) * | 2014-04-08 | 2014-06-25 | 中南大学 | In 2 O 3 ·InVO 4 Heterostructure composites and methods of making and using same |
Non-Patent Citations (1)
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|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106356291A (en) * | 2016-09-14 | 2017-01-25 | 齐鲁工业大学 | Low temperature solution method for preparing indium-titanium-oxide transparent semiconductor film |
| CN110038594A (en) * | 2019-05-13 | 2019-07-23 | 东北师范大学 | A kind of preparation method of porous oxidation indium/indium sulfide heterojunction material |
| CN115634685A (en) * | 2022-11-03 | 2023-01-24 | 常熟理工学院 | Photocatalytic material responding to visible light and preparation method thereof |
| CN115634685B (en) * | 2022-11-03 | 2023-12-08 | 常熟理工学院 | Photocatalytic material responding to visible light and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN104607170B (en) | 2017-01-18 |
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