CN103086424A - One-step synthesis method of mixed-phase titanium dioxide with exposed high-activity surfaces - Google Patents
One-step synthesis method of mixed-phase titanium dioxide with exposed high-activity surfaces Download PDFInfo
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- CN103086424A CN103086424A CN2013100621248A CN201310062124A CN103086424A CN 103086424 A CN103086424 A CN 103086424A CN 2013100621248 A CN2013100621248 A CN 2013100621248A CN 201310062124 A CN201310062124 A CN 201310062124A CN 103086424 A CN103086424 A CN 103086424A
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Abstract
The invention discloses a one-step synthesis method of mixed-phase titanium dioxide with exposed high-activity surfaces, which comprises the following steps: (1) weighing a certain amount of titanium trichloride solution, adding into distilled water, and stirring; (2) weighing a certain amount of ascorbic acid solid, adding into the solution, and stirring until the solid is completely dissolved; (3) transferring the solution into a 100mL polytetrafluoroethylene-stainless steel high-pressure reaction kettle, and reacting at 180 DEG C for 10 hours; and (4) after the reaction system is naturally cooled to room temperature, repeatedly centrifuging and washing with distilled water, placing the obtained precipitate in a vacuum drying oven, and drying at 100 DEG C for 10 hours to obtain the product. The method disclosed by the invention is simple and environment-friendly, and the time consumed in the synthesis process is short.
Description
Technical field
The present invention relates to a kind of method of one-step synthesis mixed phase and exposure high reactivity face titanium dioxide, belong to the inorganic functional material technical field.
Background technology
Due to nano titanium oxide (TiO
2) special property and potential application in environment and energy field, make it be widely studied.At present, nano titanium oxide plays an important role in fields such as photochemical catalysis, photovoltaic cell, dye sensitization solar battery and lithium ion batteries.
The performance of titanium dioxide depends on the factors such as crystalline structure, pattern, specific surface area and size.Titanium dioxide has three kinds of modal crystalline phases: anatase octahedrite (A), rutile (R) and brookite (B).These three kinds of crystalline structure are by the TiO of distortion
6The octahedra composition, difference only is its mode of connection.Result of study shows, compares with pure phase titanium dioxide, and mixed phase titanium dioxide has higher electron-hole separating power, thereby has higher photocatalytic activity.In addition, the photocatalytic activity of anatase octahedrite also has substantial connection with the active face of its exposure.{ after the titanium dioxide of 001} face, the photocatalytic activity problem that crystal face relies on has caused the extensive concern of researcher since finding to utilize hydrofluoric acid can prepare high the exposure.Yet, be difficult to large-scale application based on the method for hydrofluoric acid synthesis of titanium dioxide, because it has very large toxicity.The method of therefore, seeking simple, green synthetic exposure high-energy surface titanium dioxide remains a challenge.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of simple, green one-step synthesis mixed phase and the method for exposure high reactivity face titanium dioxide are provided.
Technical scheme of the present invention is summarized as follows:
The method of one-step synthesis mixed phase and exposure high reactivity face titanium dioxide comprises the steps:
(1) take in proportion 2.41-3.86g Titanium Trichloride Solution (massfraction is 20%, includes 3% hydrochloric acid), join in 48-76mL distilled water, stir, obtain settled solution;
(2) add the 0-0.44g xitix in step (1), at normal temperatures and pressures, continue to stir 10min, obtain settled solution;
(3) settled solution that step (2) is obtained is transferred in 100mL tetrafluoroethylene stainless steel autoclave, reacts 10h under 180 ℃;
(4) after step (3) gained suspension is cooled to room temperature, then centrifugal 10min under certain rotating speed with the distilled water washing, repeats for several times, and the gained solid is placed in dry 10h under 100 ℃ of vacuum drying ovens, namely gets product.
Preferably:
Described step (1) is: take in proportion 3.86g Titanium Trichloride Solution (massfraction is 20%, includes 3% hydrochloric acid), join in 76mL distilled water, concentration is 0.051g L
-1, stir, obtain settled solution.
Described step (2) is: add the 0.044g xitix in step (1), xitix and titanous chloride mol ratio are 0.05, at normal temperatures and pressures, continue to stir 10min, obtain settled solution.
Described step (3) is: the settled solution that step (2) is obtained is transferred in 100mL tetrafluoroethylene stainless steel autoclave, rises to 180 ℃ with the speed of 5 ℃/min from room temperature, and keep 10h at this temperature.
Described step (4) is: after step (3) gained suspension is cooled to room temperature, centrifugal 10min under the rotating speed of 4200r/min is then with distilled water washing, triplicate, the gained solid is placed in dry 10h under 100 ℃ of vacuum drying ovens, namely gets product.
Advantage of the present invention:
Raw material used in the present invention is green, method is simple, building-up process is consuming time short.The titanium dioxide that can one-step synthesis has simultaneously mixed phase and high reactivity face by regulating xitix and titanous chloride mol ratio, the nanoparticle pattern comparison rule that obtains.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.The following examples are in order to enable those skilled in the art to understand better the present invention, but the present invention are not imposed any restrictions.
Embodiment 1
The method of one-step synthesis mixed phase and exposure high reactivity face titanium dioxide comprises the steps:
(1) take 2.41g Titanium Trichloride Solution (massfraction is 20%, includes 3% hydrochloric acid), join in 48mL distilled water, stir, obtain settled solution;
(2) settled solution with step (1) gained is transferred in 100mL tetrafluoroethylene stainless steel autoclave, rises to 180 ℃ with the speed of 5 ℃/min from room temperature, and keep 10h at this temperature;
(3) after step (2) gained suspension is cooled to room temperature, centrifugal 10min under the rotating speed of 4200r/min, then with distilled water washing, triplicate is placed in dry 10h under 100 ℃ of vacuum drying ovens with the gained solid, namely gets product P 1.
Embodiment 2
The method of one-step synthesis mixed phase and exposure high reactivity face titanium dioxide comprises the steps:
(1) take 3.86g Titanium Trichloride Solution (massfraction is 20%, includes 3% hydrochloric acid), join in 76mL distilled water, stir, obtain settled solution;
(2) add the 0.044g xitix in step (1), xitix and titanous chloride mol ratio are 0.05, at normal temperatures and pressures, continue to stir 10min, obtain settled solution;
(3) settled solution that step (2) is obtained is transferred in 100mL tetrafluoroethylene stainless steel autoclave, rises to 180 ℃ with the speed of 5 ℃/min from room temperature, and keep 10h at this temperature;
(4) after step (3) gained suspension is cooled to room temperature, centrifugal 10min under the rotating speed of 4200r/min, then with distilled water washing, triplicate is placed in dry 10h under 100 ℃ of vacuum drying ovens with the gained solid, namely gets product P 2.
Embodiment 3
The method of one-step synthesis mixed phase and exposure high reactivity face titanium dioxide comprises the steps:
(1) take 3.86g Titanium Trichloride Solution (massfraction is 20%, includes 3% hydrochloric acid), join in 76mL distilled water, stir, obtain settled solution;
(2) add the 0.11g xitix in step (1), xitix and titanous chloride mol ratio are 0.125, at normal temperatures and pressures, continue to stir 10min, obtain settled solution;
(3) settled solution that step (2) is obtained is transferred in 100mL tetrafluoroethylene stainless steel autoclave, rises to 180 ℃ with the speed of 5 ℃/min from room temperature, and keep 10h at this temperature;
(4) after step (3) gained suspension is cooled to room temperature, centrifugal 10min under the rotating speed of 4200r/min, then with distilled water washing, triplicate is placed in dry 10h under 100 ℃ of vacuum drying ovens with the gained solid, namely gets product P 3.
Embodiment 4
The method of one-step synthesis mixed phase and exposure high reactivity face titanium dioxide comprises the steps:
(1) take 3.86g Titanium Trichloride Solution (massfraction is 20%, includes 3% hydrochloric acid), join in 76mL distilled water, stir, obtain settled solution;
(2) add the 0.22g xitix in step (1), xitix and titanous chloride mol ratio are 0.25, at normal temperatures and pressures, continue to stir 10min, obtain settled solution;
(3) settled solution that step (2) is obtained is transferred in 100mL tetrafluoroethylene stainless steel autoclave, rises to 180 ℃ with the speed of 5 ℃/min from room temperature, and keep 10h at this temperature;
(4) after step (3) gained suspension is cooled to room temperature, centrifugal 10min under the rotating speed of 4200r/min, then with distilled water washing, triplicate is placed in dry 10h under 100 ℃ of vacuum drying ovens with the gained solid, namely gets product P 4.
Embodiment 5
The method of one-step synthesis mixed phase and exposure high reactivity face titanium dioxide comprises the steps:
(1) take 3.86g Titanium Trichloride Solution (massfraction is 20%, includes 3% hydrochloric acid), join in 76mL distilled water, stir, obtain settled solution;
(2) add the 0.44g xitix in step (1), xitix and titanous chloride mol ratio are 0.5, at normal temperatures and pressures, continue to stir 10min, obtain settled solution;
(3) settled solution that step (2) is obtained is transferred in 100mL tetrafluoroethylene stainless steel autoclave, rises to 180 ℃ with the speed of 5 ℃/min from room temperature, and keep 10h at this temperature;
(4) after step (3) gained suspension is cooled to room temperature, centrifugal 10min under the rotating speed of 4200r/min, then with distilled water washing, triplicate is placed in dry 10h under 100 ℃ of vacuum drying ovens with the gained solid, namely gets product P 5.
The present invention relates to the technological method of a kind of one-step synthesis mixed phase and exposure high reactivity face titanium dioxide.The system of not adding xitix generates bar-shaped or granular mixed phase titanium dioxide, and along with the increase of ascorbic acid content, the ratio of anatase octahedrite increases sharply.When the mol ratio of xitix and titanous chloride was 0.05, the titanium dioxide granule that generates butt tetragonal bipyramid pattern is [this structure had more { 001} active face] at most, and { specific surface area of 001} active face can account for 18.4% of total specific surface; When the mol ratio of xitix and titanous chloride was 0.125, { specific surface area of 001} active face can account for 8.8% of total specific surface; And when xitix and titanous chloride mol ratio were 0.5, the final titanium dioxide granule that generates was vermiform, there is no { 001} active face this moment.The inventive method only need add xitix just can realize the synthetic high reactivity face titanium dioxide that exposes, simple to operate safe, nontoxic, easy to control, this greatly reduces the production cost that exposes high reactivity face titanium dioxide, is a kind of economical and practical green environmental protection technique.
Description of drawings
Fig. 1 .TiO
2The XRD of sample characterizes collection of illustrative plates: (a) P1, (b) P2, (c) P3, (d) P4 and (e) P5 (A: anatase octahedrite, R: rutile, B: brookite).
Fig. 2 .TiO
2The SEM of sample characterizes collection of illustrative plates: (a) P1, (b) P2, (c) P3 and (d) P5.
Fig. 3 .TiO
2The TEM of sample characterizes collection of illustrative plates: (a-c) P1, (d, e) P2, (f, g) P3 and (h) P5.
Claims (9)
1. the method for one-step synthesis mixed phase and exposure high reactivity face titanium dioxide, is characterized in that comprising the steps:
(1) take in proportion the 2.41-3.86g Titanium Trichloride Solution, join in 48-76mL distilled water, stir, obtain settled solution;
(2) add the 0-0.44g xitix in step (1), at normal temperatures and pressures, continue to stir 10min, obtain settled solution;
(3) settled solution that step (2) is obtained is transferred in 100mL tetrafluoroethylene stainless steel autoclave, reacts 10h under 180 ℃;
(4) after step (3) gained suspension is cooled to room temperature, then centrifugal 10min under certain rotating speed with the distilled water washing, repeats for several times, and the gained solid is placed in dry 10h under 100 ℃ of vacuum drying ovens, namely gets product.
2. method according to claim 1, it is characterized in that described in described step (1): the Titanium Trichloride Solution massfraction is 20%, includes 3% hydrochloric acid.
3. method according to claim 1, is characterized in that described in described step (1): take in proportion the 3.86g Titanium Trichloride Solution, join in 76mL distilled water, stir, obtain settled solution.
4. method according to claim 1 is characterized in that described in described step (2): do not add xitix, at normal temperatures and pressures, continue to stir 10min, obtain settled solution, the finished product are bar-shaped or granular mixed phase titanium dioxide.
5. method according to claim 1, it is characterized in that described in described step (2): add the 0.044g xitix in step (1), xitix and titanous chloride mol ratio are 0.05, at normal temperatures and pressures, continue to stir 10min, obtain settled solution, the titanium dioxide granule of the final butt tetragonal bipyramid pattern that generates is maximum, and { specific surface area of 001} active face accounts for 18.4% of the total specific surface of titanium dioxide granule at this moment.
6. method according to claim 1, it is characterized in that described in described step (2): add the 0.11g xitix in step (1), xitix and titanous chloride mol ratio are 0.125, at normal temperatures and pressures, continue to stir 10min, obtain settled solution, have the titanium dioxide granule of butt tetragonal bipyramid pattern in the finished product, { specific surface area of 001} active face accounts for 8.8% of the total specific surface of titanium dioxide granule.
7. method according to claim 1, it is characterized in that described in described step (2): add the 0.44g xitix in step (1), xitix and titanous chloride mol ratio are 0.5, at normal temperatures and pressures, continue to stir 10min, obtain settled solution, the final titanium dioxide granule that generates is vermiform, there is no { 001} active face this moment.
8. method according to claim 1, it is characterized in that described in described step (3): the settled solution that step (2) is obtained is transferred in 100mL tetrafluoroethylene stainless steel autoclave, speed with 5 ℃/min rises to 180 ℃ from room temperature, and keeps 10h at this temperature.
9. method according to claim 1, it is characterized in that described in described step (4): after step (3) gained suspension is cooled to room temperature, centrifugal 10min under the rotating speed of 4200r/min, then wash with distilled water, triplicate, the gained solid is placed in dry 10h under 100 ℃ of vacuum drying ovens, namely gets product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103553124A (en) * | 2013-11-08 | 2014-02-05 | 中国科学技术大学 | Method for preparing blue titanium dioxide |
| CN110342573A (en) * | 2019-07-17 | 2019-10-18 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of cube titanium oxide |
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| CN102515270A (en) * | 2011-12-13 | 2012-06-27 | 武汉大学 | Preparation method of mixed crystal-type nanoscale TiO2 having exposed (001) crystal faces |
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| SOPHIE CASSAIGNON ET AL.: "From TiCl3 to TiO2 nanoparticles（anatase，brookite and rutile）：Thermohydrolysis and oxidation in aqueous medium", 《JOURNAL OF PHYSICS AND CHEMISTRY OF SOLIDS》, vol. 68, 31 December 2007 (2007-12-31), pages 695 - 700 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553124A (en) * | 2013-11-08 | 2014-02-05 | 中国科学技术大学 | Method for preparing blue titanium dioxide |
| CN103553124B (en) * | 2013-11-08 | 2015-03-11 | 中国科学技术大学 | Method for preparing blue titanium dioxide |
| CN110342573A (en) * | 2019-07-17 | 2019-10-18 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of cube titanium oxide |
| CN110342573B (en) * | 2019-07-17 | 2021-08-03 | 中国科学院宁波材料技术与工程研究所 | Preparation method of cubic titanium oxide |
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