CN104229878A - Preparation method of rutile crystal-form titanium dioxide nanorod - Google Patents
Preparation method of rutile crystal-form titanium dioxide nanorod Download PDFInfo
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- CN104229878A CN104229878A CN201410442352.2A CN201410442352A CN104229878A CN 104229878 A CN104229878 A CN 104229878A CN 201410442352 A CN201410442352 A CN 201410442352A CN 104229878 A CN104229878 A CN 104229878A
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- titanium dioxide
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Abstract
The invention discloses a preparation method of a rutile crystal-form titanium dioxide nanorod. The nanorod is a rutile crystal-form titanium dioxide nanorod, wherein the nanorod is 100-120nm long, and the diameter of the nanorod is 20-50nm. The preparation method comprises the following steps: dissolving a titanium trichloride crystal in water in a weight ratio of 2.5%-5%, and then stirring to obtain a titanium trichloride aqueous solution; placing the solution in a sealed state, reacting for at least 25-70 hours at a temperature of 100-120 DEG C to obtain a reaction liquid; and washing precipitated in the cooled reaction liquid with distilled water, and then drying to obtain target products. The rutile crystal-form titanium dioxide nanorod has the performance of absorbing visible light and can be widely applied to the fields such as solar cells and photocatalysis.
Description
technical field:
The present invention relates to titanium dioxide process, especially relate to a kind of preparation method of rutile crystal type titanium dioxide nano-rod.
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background technology:
Semi-conductor titanium dioxide is as a kind of cheap effective photocatalyst, and its preparation and performance study get more and more people's extensive concerning.Anatase octahedrite and rutile are two kinds of important crystalline phases of titanium dioxide.Anatase octahedrite is widely used in photocatalysis field due to the photocatalytic activity had.With Anatase ratio, although rutile photo-catalysis capability is not high, because it has better physical and chemical stability, high optical index, very strong opacifying power and tinting strength, be widely used in multiple fields such as optical material research, coating, makeup.The synthetic method of tradition red schorl phase titanium dioxide ultrafine particle mainly contains sol-gel method, microemulsion method, high temperature gas-phase reaction method etc., wherein sol-gel, microemulsion method production cost are high, long reaction time, and first reaction will generate unformed TiO2, need could obtain the particle of Rutile Type through high temperature (800-1000 DEG C) calcining, calcination process very easily causes particle aggregation and sintering; High temperature gas phase method directly can obtain rutile particle, speed of response is fast, can realize continuous seepage, but reacts complete instantaneous when high temperature, require material microcosmic mixing within the extremely short time, have very high requirement to type of reactor, material, heating means and feeding manner.
In prior art with organic titanium or inorganic titanium for raw material, just can obtain red schorl phase titanium dioxide without pyroprocessing, but there is complicated operation, the problem such as product is easily reunited, crystallization degree is bad.
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summary of the invention:
The present invention is directed to the technical problem that prior art exists, adopt low-temperature hydrothermal production method, propose a kind of preparation method of rutile crystal type titanium dioxide nano-rod.
Technical scheme of the present invention is:
A preparation method for rutile crystal type titanium dioxide nano-rod, preparation is carried out in accordance with the following steps:
1) dissolve purple titanium trichloride xln with distilled water, make the titanium trichloride aqueous solution that mass percent concentration is 2.5%;
2) step 1 gained solution being heated in a kettle. temperature is react 25 ~ 50h, cool to room temperature at 120 DEG C ~ 150 DEG C;
3) after the throw out in reaction solution being filtered, with distilled water wash for several times, after centrifuge dehydration at 90 DEG C dry 2h, obtained rutile crystal type titanium dioxide nano-rod.
Obtained rutile crystal type titanium dioxide nano-rod is that the rod length of nanometer rod is 100 ~ 120nm, excellent diameter is 20 ~ 50nm by the rhabdolith of a lot of needle-like thin brilliant comparison rule of assembling.
Drying process in preparation process, uses the too low drying temperature being less than 90 DEG C to extend time of drying, consequently causes the hard aggregation of photocatalyst granular, reduce the photocatalytic activity of product.
The titanium trichloride aqueous solution concentration used in preparation process, have influence on the formation crystal formation of nano titanium oxide, the aqueous solution lower than the mass percent concentration of 5% is conducive to the formation of Rutile Type.
In preparation process, the pattern of temperature and time to the crystal grain of nano titanium oxide of hydro-thermal reaction has material impact, and improve the formation that temperature is conducive to rutile titanium dioxide rhabdolith, simultaneous temperature is higher, and the reaction times wants corresponding shortening.
The invention has the beneficial effects as follows and adopt the preparation method of low-temperature hydrothermal to efficiently avoid high-temperature calcination process, obtain high, the evengranular nanoclub-like crystal of crystallization degree, and well remain surface tissue and the surface hydroxyl of catalyzer, be conducive to the compound reducing photohole and electronics, thus make red schorl phase titanium dioxide nano powder obtain higher catalytic activity.
embodiment:
Specific embodiments of the invention:
Embodiment 1:
A preparation method for rutile crystal type titanium dioxide nano-rod, preparation is carried out in accordance with the following steps:
1) dissolve purple titanium trichloride xln with distilled water, make the titanium trichloride aqueous solution that mass percent concentration is 2.5%;
2) step 1 gained solution is heated in a kettle. at temperature is 120 DEG C and reacts 50h, cool to room temperature;
3) after the throw out in reaction solution being filtered, with distilled water wash for several times, after centrifuge dehydration at 90 DEG C dry 2h, obtained rutile crystal type titanium dioxide nano-rod.
Embodiment 2:
A preparation method for rutile crystal type titanium dioxide nano-rod, preparation is carried out in accordance with the following steps:
1) dissolve purple titanium trichloride xln with distilled water, make the titanium trichloride aqueous solution that mass percent concentration is 2.5%;
2) step 1 gained solution is heated in a kettle. at temperature is 150 DEG C and reacts 25h, cool to room temperature;
3) after the throw out in reaction solution being filtered, with distilled water wash for several times, after centrifuge dehydration at 90 DEG C dry 2h, obtained rutile crystal type titanium dioxide nano-rod.
Claims (3)
1. a preparation method for rutile crystal type titanium dioxide nano-rod, is characterized in that, preparation is carried out in accordance with the following steps:
1) dissolve purple titanium trichloride xln with distilled water, make the titanium trichloride aqueous solution that mass percent concentration is 2.5%;
2) step 1 gained solution being heated in a kettle. temperature is react 25 ~ 50h, cool to room temperature at 120 DEG C ~ 150 DEG C;
3) after the throw out in reaction solution being filtered, with distilled water wash for several times, after centrifuge dehydration at 90 DEG C dry 2h, obtained rutile crystal type titanium dioxide nano-rod.
2. according to the preparation method of a kind of rutile crystal type titanium dioxide nano-rod described in claim 1, it is characterized in that, preparation is carried out in accordance with the following steps:
1) dissolve purple titanium trichloride xln with distilled water, make the titanium trichloride aqueous solution that mass percent concentration is 2.5%;
2) step 1 gained solution is heated in a kettle. at temperature is 120 DEG C and reacts 50h, cool to room temperature;
3) after the throw out in reaction solution being filtered, with distilled water wash for several times, after centrifuge dehydration at 90 DEG C dry 2h, obtained rutile crystal type titanium dioxide nano-rod.
3. according to the preparation method of a kind of rutile crystal type titanium dioxide nano-rod described in claim 1, it is characterized in that, preparation is carried out in accordance with the following steps:
1) dissolve purple titanium trichloride xln with distilled water, make the titanium trichloride aqueous solution that mass percent concentration is 2.5%;
2) step 1 gained solution is heated in a kettle. at temperature is 150 DEG C and reacts 25h, cool to room temperature;
3) after the throw out in reaction solution being filtered, with distilled water wash for several times, after centrifuge dehydration at 90 DEG C dry 2h, obtained rutile crystal type titanium dioxide nano-rod.
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| CN201410442352.2A CN104229878A (en) | 2014-09-02 | 2014-09-02 | Preparation method of rutile crystal-form titanium dioxide nanorod |
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| CN201410442352.2A CN104229878A (en) | 2014-09-02 | 2014-09-02 | Preparation method of rutile crystal-form titanium dioxide nanorod |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883829A (en) * | 2017-04-20 | 2017-06-23 | 济南大学 | A kind of regulatable TiO2Composite aqueous nano-fluids of-Au and preparation method thereof |
| CN107814412A (en) * | 2017-12-11 | 2018-03-20 | 南京工业大学 | A kind of particle morphology is the synthetic method of bar-shaped rutile type nano titanic oxide |
| CN111634943A (en) * | 2020-06-15 | 2020-09-08 | 上海工程技术大学 | Crystalline phase regulation and control method of titanium dioxide nano material |
| CN115106073A (en) * | 2022-05-20 | 2022-09-27 | 深圳大学 | Titanium hydroxide doped nanorod with photocatalytic hydrogen production function and preparation method and application thereof |
-
2014
- 2014-09-02 CN CN201410442352.2A patent/CN104229878A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 赵晓红等: "低温水热法制备高活性纳米金红石相二氧化钛", 《化学研究与应用》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883829A (en) * | 2017-04-20 | 2017-06-23 | 济南大学 | A kind of regulatable TiO2Composite aqueous nano-fluids of-Au and preparation method thereof |
| CN106883829B (en) * | 2017-04-20 | 2019-10-11 | 济南大学 | A kind of regulatable TiO2Composite aqueous nano-fluid of-Au and preparation method thereof |
| CN107814412A (en) * | 2017-12-11 | 2018-03-20 | 南京工业大学 | A kind of particle morphology is the synthetic method of bar-shaped rutile type nano titanic oxide |
| CN111634943A (en) * | 2020-06-15 | 2020-09-08 | 上海工程技术大学 | Crystalline phase regulation and control method of titanium dioxide nano material |
| CN111634943B (en) * | 2020-06-15 | 2022-08-23 | 上海工程技术大学 | Crystalline phase regulation and control method of titanium dioxide nano material |
| CN115106073A (en) * | 2022-05-20 | 2022-09-27 | 深圳大学 | Titanium hydroxide doped nanorod with photocatalytic hydrogen production function and preparation method and application thereof |
| CN115106073B (en) * | 2022-05-20 | 2024-03-29 | 深圳大学 | Titanium hydroxide nano-rod doped with hydrogen produced by photocatalysis as well as preparation method and application thereof |
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Application publication date: 20141224 |