CN104229879A - Preparation method of rutile titanium dioxide nano powder - Google Patents
Preparation method of rutile titanium dioxide nano powder Download PDFInfo
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- CN104229879A CN104229879A CN201410442404.6A CN201410442404A CN104229879A CN 104229879 A CN104229879 A CN 104229879A CN 201410442404 A CN201410442404 A CN 201410442404A CN 104229879 A CN104229879 A CN 104229879A
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Abstract
The invention discloses a preparation method of rutile titanium dioxide nano powder. The invention provides a simple low-temperature hydrothermal process aiming at such problems of the existing low-temperature rutile titanium dioxide nano powder as complicated operation and poor crystallization degree. The method comprises the following steps: heating a titanium trichloride water solution with mass percent concentration being 2.5%-5% of to 70-100 DEG C in a reaction kettle and reacting for 50 hours; and filtering sediment, centrifugally dewatering and drying the sediment at 90 DEG C for 2 hours, so as to prepare the rutile titanium dioxide nano powder. The prepared rutile titanium dioxide nano powder is regular acicular crystal which is an aggregation of a plurality of fine acicular crystals, and is good in crystal degree, regular in shape, and small in particle, and the size is about 20*100nm. According to the preparation method, a high-temperature roasting process is avoided, and the surface structure and surface hydroxyl group of the catalyst are reserved, so that the titanium dioxide nano powder has high catalytic activity.
Description
technical field:
The present invention relates to titanic oxide nano and preparation method thereof, especially relate to a kind of preparation method of red schorl phase titanium dioxide nano powder.
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.
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 red schorl phase titanium dioxide nano powder, preparation method thereof.
Technical scheme of the present invention is:
A kind of red schorl phase titanium dioxide nano powder, preparation method thereof, comprises the following steps:
1) dissolve purple titanium trichloride xln with distilled water, making mass percent concentration is stir 30 minutes after the titanium trichloride aqueous solution of 2.5% ~ 5%;
2) step 1 gained solution being heated in a kettle. temperature is react 50h at 70 DEG C ~ 100 DEG C, adds strong mixing, cool to room temperature simultaneously;
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 red schorl phase titanium dioxide nano powder.
Obtained red schorl phase titanium dioxide nano powder is that crystal degree is good, pattern is regular, particle is less, and size is approximately 20 × 100nm by the needle-like crystal of a lot of needle-like thin brilliant comparison rule of assembling.
Found through experiments, in preparation process, stirring power affects the shape of nano particle, and under agitation, the particle of acquisition is less, and shape is more regular.
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, 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 nanocrystal 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 kind of red schorl phase titanium dioxide nano powder, preparation method thereof, comprises the following steps:
1) dissolve purple titanium trichloride xln with distilled water, making mass percent concentration is stir 30 minutes after the titanium trichloride aqueous solution of 2.5%;
2) step 1 gained solution is heated in a kettle. at temperature is 70 DEG C and reacts 50h, add strong mixing, cool to room temperature simultaneously;
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 red schorl phase titanium dioxide nano powder.
Embodiment 2:
A kind of red schorl phase titanium dioxide nano powder, preparation method thereof, comprises the following steps:
1) dissolve purple titanium trichloride xln with distilled water, making mass percent concentration is stir 30 minutes after the titanium trichloride aqueous solution of 3%;
2) step 1 gained solution is heated in a kettle. at temperature is 70 DEG C and reacts 50h, add strong mixing, cool to room temperature simultaneously;
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 red schorl phase titanium dioxide nano powder.
Embodiment 3:
A kind of red schorl phase titanium dioxide nano powder, preparation method thereof, comprises the following steps:
1) dissolve purple titanium trichloride xln with distilled water, making mass percent concentration is stir 30 minutes after the titanium trichloride aqueous solution of 4%;
2) step 1 gained solution is heated in a kettle. at temperature is 70 DEG C and reacts 50h, add strong mixing, cool to room temperature simultaneously;
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 red schorl phase titanium dioxide nano powder.
Embodiment 4:
A kind of red schorl phase titanium dioxide nano powder, preparation method thereof, comprises the following steps:
1) dissolve purple titanium trichloride xln with distilled water, making mass percent concentration is stir 30 minutes after the titanium trichloride aqueous solution of 5%;
2) step 1 gained solution is heated in a kettle. at temperature is 70 DEG C and reacts 50h, add strong mixing, cool to room temperature simultaneously;
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 red schorl phase titanium dioxide nano powder.
Embodiment 5:
A kind of red schorl phase titanium dioxide nano powder, preparation method thereof, comprises the following steps:
1) dissolve purple titanium trichloride xln with distilled water, making mass percent concentration is stir 30 minutes after the titanium trichloride aqueous solution of 2.5%;
2) step 1 gained solution is heated in a kettle. at temperature is 100 DEG C and reacts 50h, add strong mixing, cool to room temperature simultaneously;
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 red schorl phase titanium dioxide nano powder.
Claims (2)
1. a red schorl phase titanium dioxide nano powder, preparation method thereof, is characterized in that, preparation is carried out in accordance with the following steps:
1) dissolve purple titanium trichloride xln with distilled water, making mass percent concentration is stir 30 minutes after the titanium trichloride aqueous solution of 2.5% ~ 5%;
2) step 1 gained solution being heated in a kettle. temperature is react 50h at 70 DEG C ~ 100 DEG C, adds strong mixing, cool to room temperature simultaneously;
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 red schorl phase titanium dioxide nano powder.
2. according to a kind of red schorl phase titanium dioxide nano powder, preparation method thereof 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, making mass percent concentration is stir 30 minutes after the titanium trichloride aqueous solution of 2.5%;
2) step 1 gained solution is heated in a kettle. at temperature is 100 DEG C and reacts 50h, add strong mixing, cool to room temperature simultaneously;
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 red schorl phase titanium dioxide nano powder.
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| CN201410442404.6A CN104229879A (en) | 2014-09-02 | 2014-09-02 | Preparation method of rutile titanium dioxide nano powder |
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| CN201410442404.6A CN104229879A (en) | 2014-09-02 | 2014-09-02 | Preparation method of rutile titanium dioxide nano powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112852163A (en) * | 2019-11-12 | 2021-05-28 | 中国科学院化学研究所 | Crystalline nanoparticle, photocurable organic silicon resin and nanoparticle composition, preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3650693A (en) * | 1970-09-24 | 1972-03-21 | Du Pont | Preparation of fibrous titanium dioxide |
| CN102701277A (en) * | 2012-06-18 | 2012-10-03 | 山东轻工业学院 | Method for preparing rutile titanium dioxide |
| CN103539202A (en) * | 2013-08-23 | 2014-01-29 | 中山大学 | Method for preparing titanium dioxide nanowire through self-reaction of single reagent |
-
2014
- 2014-09-02 CN CN201410442404.6A patent/CN104229879A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3650693A (en) * | 1970-09-24 | 1972-03-21 | Du Pont | Preparation of fibrous titanium dioxide |
| CN102701277A (en) * | 2012-06-18 | 2012-10-03 | 山东轻工业学院 | Method for preparing rutile titanium dioxide |
| CN103539202A (en) * | 2013-08-23 | 2014-01-29 | 中山大学 | Method for preparing titanium dioxide nanowire through self-reaction of single reagent |
Non-Patent Citations (2)
| Title |
|---|
| WANG HEQUAN ET AL.: "Tunable synthesis of hierarchical TiO2 spheres consisting of rutile nanowires for dye-sensitized solar cells and photocatalysis", 《CRYST.RES.TECHNOL》 * |
| 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112852163A (en) * | 2019-11-12 | 2021-05-28 | 中国科学院化学研究所 | Crystalline nanoparticle, photocurable organic silicon resin and nanoparticle composition, preparation method and application |
| CN112852163B (en) * | 2019-11-12 | 2022-05-03 | 中国科学院化学研究所 | Crystalline nanoparticle, photocurable organic silicon resin and nanoparticle composition, preparation method and application |
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Application publication date: 20141224 |