CN104607169A - Preparation method and application of In2TiO5 - Google Patents
Preparation method and application of In2TiO5 Download PDFInfo
- Publication number
- CN104607169A CN104607169A CN201510004886.1A CN201510004886A CN104607169A CN 104607169 A CN104607169 A CN 104607169A CN 201510004886 A CN201510004886 A CN 201510004886A CN 104607169 A CN104607169 A CN 104607169A
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- tio
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Abstract
The invention discloses a preparation method and an application of In2TiO5. The preparation method comprises the steps of taking glycine, indium nitrate and butyl titanate as raw materials, wherein the mole ratio of indium nitrate to butyl titanate is 2:1, and carrying out high-temperature roasting. A synthesis condition is mild, and synthesized In2TiO5 is stable in performance, high in activity and reusable. In2TiO5 is applied to photocatalytic degradation of quinolone antibiotics for the first time, and has relatively high photocatalysis efficiency on an antibiotic contaminant, namely levofloxacin hydrochloride under ultraviolet irradiation.
Description
Technical field
The invention belongs to technical field of material, be specifically related to In
2tiO
5preparation method, also relate to In
2tiO
5application.
Background technology
Sanitary sewage and part trade effluent applicable biological method are effectively processed, but the degraded of difficult for biological degradation, toxic compounds must be sought effective, suitable method and processes.Large quantifier elimination shows, photocatalytic method can effectively by organic pollutant degradations such as agricultural chemicals, antibiotics, phenols and aromatic hydrocarbons, and final mineralising is CO
2, H
2the material that O etc. are nontoxic, reaches the object eliminating organic pollution completely.Titanate nano material has higher mechanical performance, excellent physical property, preferably heat endurance and chemical stability, excellent electric property and optical property, occupies very important position in contemporary material science.In
2tiO
5by [InO
6] and [TiO
6] octahedron composition orthorhombic system composite oxide of metal, have three-dimensional tunnel structure, energy gap is about 3.02 ~ 3.20ev.In is prepared in prior art
2tiO
5method technological requirement harsh, also not by In
2tiO
5for the research in photocatalysis.
Summary of the invention
The object of this invention is to provide In
2tiO
5preparation method, solve the preparation In existed in prior art
2tiO
5the technical problem of method technological requirement harshness.
Another object of the present invention is to provide according to above-mentioned In
2tiO
5the In for preparing of preparation method
2tiO
5application.
The first technical scheme that the present invention adopts is, In
2tiO
5preparation method, specifically 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: yellow solution c is placed in 130 DEG C ~ 140 DEG C oil baths and evaporates, until solution becomes Tan solid, stops heating;
Step 5: foam Tan solid at 180 DEG C ~ 220 DEG C 30 ~ 60min, obtains yellowish-brown powder, and by yellowish-brown powder transfer in ceramic crucible;
Step 6: ceramic crucible is placed in Muffle furnace, 200 DEG C ~ 300 DEG C are warming up to 5 DEG C/min, constant temperature 30 ~ 60min, 400 DEG C ~ 500 DEG C are warming up to again with 2 DEG C/min, constant temperature 30 ~ 60min, is finally warming up to 700 ~ 1000 DEG C with 10 DEG C/min, constant temperature 0 ~ 6h, naturally cool to room temperature, obtain white In
2tiO
5powder.
The feature of the first 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.
Another technical scheme of the present invention is, according to above-mentioned In
2tiO
5the In for preparing of preparation method
2tiO
5application, it is used as the photochemical catalyst of ultraviolet degradation lavo-ofloxacin.
The invention has the beneficial effects as follows, first by In
2tiO
5be applied to photocatalytic degradation carbostyril antibiotic, under UV-irradiation, to antibiotic contamination lavo-ofloxacin hydrochloride, there is higher photocatalysis efficiency.The present invention prepares In
2tiO
5method synthesis condition gentle, the In of synthesis
2tiO
5stable performance, active high, reusable.
Accompanying drawing illustrates:
Fig. 1 is photochemical catalyst In prepared by the inventive method
2tiO
5xRD figure.
Fig. 2 is photochemical catalyst In prepared by the inventive method
2tiO
5absorbance change curve (a) of catalytic degradation lavo-ofloxacin and c
0/ c
t-t curve (b), experiment condition is: light source is 125W mercury lamp, and reactant liquor is the lavo-ofloxacin hydrochloride solution 50mL of 20mg/L, and the addition of 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.
The present invention prepares photochemical catalyst 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, slowly drop 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: yellow solution c is placed in 130 DEG C ~ 140 DEG C oil baths and evaporates, until solution becomes Tan solid, stops heating;
Step 5: foam Tan solid at 180 DEG C ~ 220 DEG C 30 ~ 60min, obtains yellowish-brown powder, and by yellowish-brown powder transfer in ceramic crucible;
Step 6: ceramic crucible is placed in Muffle furnace, 200 DEG C ~ 300 DEG C are warming up to 5 DEG C/min, constant temperature 30 ~ 60min, 400 DEG C ~ 500 DEG C are warming up to again with 2 DEG C/min, constant temperature 30 ~ 60min, is finally warming up to 700 ~ 1000 DEG C with 10 DEG C/min, constant temperature 0 ~ 6h, naturally cool to room temperature, obtain white In
2tiO
5powder.
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), this illustrates that this photochemical catalyst is In
2tiO
5.
Known see Fig. 2, after mercury lamp irradiation 180min, add photochemical catalyst In
2tiO
5when not adding photochemical catalyst, the clearance difference 71.8%, 14.7% of lavo-ofloxacin, this shows, this photochemical catalyst shows good catalytic activity under ultraviolet light.
The present invention is first by In
2tiO
5be applied to photocatalytic degradation carbostyril antibiotic, its under UV-irradiation to water body in antibiotic contamination lavo-ofloxacin hydrochloride there is higher photocatalysis efficiency.The present invention prepares In
2tiO
5method synthesis condition gentle, the In of synthesis
2tiO
5stable performance, active high, reusable.
Example 1
0.1125g glycine solid is configured to the ethylene glycol solution of 0.2wt%, 75 DEG C of water bath with thermostatic control lower magnetic forces stir 40min, 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, it is slowly dropped in solution a with the speed of 20/min, then under 85 DEG C of waters bath with thermostatic control in magnetic agitation 40min, obtain solution b; The butyl titanate of 0.17g 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; Then yellow solution c is placed in 130 DEG C of oil baths to evaporate, until solution becomes Tan solid, stops heating; Foam Tan solid at 200 DEG C 30min, obtains yellowish-brown powder, and by yellowish-brown powder transfer in ceramic crucible; Finally ceramic crucible is placed in Muffle furnace, is warming up to 300 DEG C with 5 DEG C/min, constant temperature 30min, then be warming up to 500 DEG C with 2 DEG C/min, constant temperature 30min, be finally warming up to 900 DEG C with 10 DEG C/min, constant temperature 1h, naturally cools to room temperature, obtains white In
2tiO
5powder.
Example 2
0.55g glycine solid is configured to the ethylene glycol solution of 0.3wt%, 85 DEG C of water bath with thermostatic control lower magnetic forces stir 30min, 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, it is slowly dropped in solution a with the speed of 25/min, then under 75 DEG C of waters bath with thermostatic control in magnetic agitation 60min, obtain solution b; 0.8311g butyl titanate is slowly dropped in solution b with the speed of 30/min, then magnetic agitation 90min in 85 DEG C of waters bath with thermostatic control, stop heating water bath, obtain yellow solution c; Then yellow solution c is placed in 140 DEG C of oil baths to evaporate, until solution becomes Tan solid, stops heating; By Tan solid at the 60min that foamed at 180 DEG C by Tan solid, obtain yellowish-brown powder, and by yellowish-brown 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 40min, then be warming up to 450 DEG C with 2 DEG C/min, constant temperature 40min, be finally warming up to 800 DEG C with 10 DEG C/min, constant temperature 2h, naturally cools to room temperature, obtains white In
2tiO
5powder.
Example 3
1.3g glycine solid is configured to the ethylene glycol solution of 0.5wt%, 80 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)
3be dissolved in ethylene glycol, be made into the In (NO that concentration is 0.3mol/L
3)
3ethylene glycol solution, it is slowly dropped in solution a with the speed of 30/min, then under 80 DEG C of waters bath with thermostatic control in magnetic agitation 30min, obtain solution b; 1.9644g butyl titanate is slowly dropped in solution b with the speed of 25/min, then magnetic agitation 150min in 75 DEG C of waters bath with thermostatic control, stop heating water bath, obtain yellow solution c; Then yellow solution c is placed in 135 DEG C of oil baths to evaporate, until solution becomes Tan solid, stops heating; By Tan solid at the 40min that foamed at 220 DEG C by Tan solid, obtain yellowish-brown powder, and by yellowish-brown 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 60min, then be warming up to 400 DEG C with 2 DEG C/min, constant temperature 60min, be finally warming up to 700 DEG C with 10 DEG C/min, constant temperature 6h, naturally cools to room temperature, obtains white In
2tiO
5powder.
Example 4
2.1g glycine solid is configured to the ethylene glycol solution of 0.4wt%, 80 DEG C of water bath with thermostatic control lower magnetic forces stir 50min, obtain clear transparent solutions a; By the In (NO of 7.1269g
3)
3be dissolved in ethylene glycol, be made into the In (NO that concentration is 0.15mol/L
3)
3ethylene glycol solution, it is slowly dropped in solution a with the speed of 20/min, then under 80 DEG C of waters bath with thermostatic control in magnetic agitation 50min, obtain solution b; 3.17g butyl titanate is slowly dropped in solution b with the speed of 20/min, then magnetic agitation 100min in 80 DEG C of waters bath with thermostatic control, stop heating water bath, obtain yellow solution c; Then yellow solution c is placed in 140 DEG C of oil baths to evaporate, until solution becomes Tan solid, stops heating; By Tan solid at the 50min that foamed at 190 DEG C by Tan solid, obtain yellowish-brown powder, and by yellowish-brown 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 50min, then be warming up to 400 DEG C with 2 DEG C/min, constant temperature 50min, be finally warming up to 1000 DEG C with 10 DEG C/min and naturally cool to room temperature immediately, obtain white In
2tiO
5powder.
Claims (5)
1.In
2tiO
5preparation method, it is characterized in that, specifically 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: yellow solution c is placed in 130 DEG C ~ 140 DEG C oil baths and evaporates, until solution becomes Tan solid, stops heating;
Step 5: foam Tan solid at 180 DEG C ~ 220 DEG C 30 ~ 60min, obtains yellowish-brown powder, and by yellowish-brown powder transfer in ceramic crucible;
Step 6: ceramic crucible is placed in Muffle furnace, 200 DEG C ~ 300 DEG C are warming up to 5 DEG C/min, constant temperature 30 ~ 60min, 400 DEG C ~ 500 DEG C are warming up to again with 2 DEG C/min, constant temperature 30 ~ 60min, is finally warming up to 700 ~ 1000 DEG C with 10 DEG C/min, constant temperature 0 ~ 6h, naturally cool to room temperature, obtain white In
2tiO
5powder.
2. according to claim 1
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.
3. according to claim 1
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.
4. according to claim 1
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.
5. the according to any one of Claims 1-4
2tiO
5the In for preparing of preparation method
2tiO
5application, it is characterized in that, it is used as the photochemical catalyst of ultraviolet degradation lavo-ofloxacin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510004886.1A CN104607169A (en) | 2015-01-06 | 2015-01-06 | Preparation method and application of In2TiO5 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510004886.1A CN104607169A (en) | 2015-01-06 | 2015-01-06 | Preparation method and application of In2TiO5 |
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| Publication Number | Publication Date |
|---|---|
| CN104607169A true CN104607169A (en) | 2015-05-13 |
Family
ID=53141973
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|---|---|---|---|
| CN201510004886.1A Pending CN104607169A (en) | 2015-01-06 | 2015-01-06 | Preparation method and application of In2TiO5 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105107492A (en) * | 2015-07-28 | 2015-12-02 | 榆林学院 | Quasi-one dimensional In2TiO5 nanobelt and preparation method thereof |
| CN108704380A (en) * | 2018-05-29 | 2018-10-26 | 沈阳理工大学 | A kind of preparation method of water process porcelain sand filter material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
| US20140271916A1 (en) * | 2013-03-15 | 2014-09-18 | Nitto Denko Corporation | Multivalence photocatalytic semiconductor elements |
-
2015
- 2015-01-06 CN CN201510004886.1A patent/CN104607169A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
| US20140271916A1 (en) * | 2013-03-15 | 2014-09-18 | Nitto Denko Corporation | Multivalence photocatalytic semiconductor elements |
Non-Patent Citations (2)
| Title |
|---|
| YUAN LIU等: ""Higher visible photocatalytic activities of nitrogen doped In2TiO5 sensitized by carbon nitride"", 《JOURNAL OF HAZARDOUS MATERIALS》 * |
| 米晓云等: "《Al2O3纳米粉体及透明陶瓷》", 31 March 2012 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105107492A (en) * | 2015-07-28 | 2015-12-02 | 榆林学院 | Quasi-one dimensional In2TiO5 nanobelt and preparation method thereof |
| CN108704380A (en) * | 2018-05-29 | 2018-10-26 | 沈阳理工大学 | A kind of preparation method of water process porcelain sand filter material |
| CN108704380B (en) * | 2018-05-29 | 2020-08-04 | 沈阳理工大学 | Preparation method of porcelain sand filter material for water treatment |
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Application publication date: 20150513 |