CN102583526A - Preparation method of titanium dioxide classification balls containing three crystalline phases - Google Patents
Preparation method of titanium dioxide classification balls containing three crystalline phases Download PDFInfo
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- CN102583526A CN102583526A CN2012100227482A CN201210022748A CN102583526A CN 102583526 A CN102583526 A CN 102583526A CN 2012100227482 A CN2012100227482 A CN 2012100227482A CN 201210022748 A CN201210022748 A CN 201210022748A CN 102583526 A CN102583526 A CN 102583526A
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Abstract
The invention discloses a preparation method of titanium dioxide classification balls containing three crystalline phases. The method comprises the following steps that: 0.25g-0.3g of analytically-pure dodecyltrimethylammonium bromide is added into a mixed solvent containing 30ml of absolute ethyl alcohol and 30ml of deionized water to be mixed uniformly, 0.4ml-0.8ml of analytically-pure tartaric acid is added then, and all the materials are stirred and mixed uniformly at a normal temperature to obtain a mixed solution; 1ml-2ml of analytically-pure tetrabutyl orthotitanate is dropwise added into the mixed solution and is continually stirred till white flocs disappear; the generated solution is transferred into a high-temperature reaction kettle of 100ml; the reaction kettle is put into a constant-temperature drying oven to be subjected to heat insulation at a temperature of 120-150 DEG C for 24 hours to 48 hours, and then is cooled to a room temperature to obtain white precipitates; and the white precipitates are washed repeatedly for 2-3 times by deionized water or absolute ethyl alcohol, and then are dried in the drying oven at a temperature of 60-80 DEG C for 10 hours to12 hours. According to the invention, the cost is low, the technical control process is simple, and the large-scale synthesis is easy.
Description
Technical field
The present invention relates to a kind of preparation method who contains three kinds of crystalline phase titanium oxide classification balls.
Background technology
Titanium oxide enjoys the parent of industry member and academia to look at because of it in extensive applications such as the environment and the energy as a kind of important function property oxide semiconductor material.In order to adapt to the application of titanium oxide under different occasions, studies obtains the common concern of academia like the microscopic appearance of control titanium oxide crystalline phase and control titanium oxide etc.
In the Control Study that relates to the titanium oxide crystalline phase, at present report has pure rutile type titanium oxide, pure anatase titanium dioxide, pure brookite type titanium dioxide and above-mentioned mixed phase and three phase titanic oxides synthetic.In the research of exploring the titanium oxide microscopic appearance, mainly comprise monodimension nanometer material and have the nano material of classification spherical structure.Titanium oxide with classification spherical structure is big because of its some particular performances such as specific surface area, and scattering of light waits by force and is used widely.Although aspect the control and microstructural regulation and control of crystalline phase, synthetic some progress that obtained about titanium oxide combine synthesizing of three kinds of crystalline phases and classification ball microscopic appearance to rarely have report.
Summary of the invention
The object of the present invention is to provide the preparation method that a kind of low cost, technological process are simple, mass preparation contains three kinds of crystalline phase titanium oxide classification balls, promptly adopt the solvent-thermal method preparation to contain the preparation method of three kinds of crystalline phase titanium oxide classification balls.
Concrete steps are:
(1) 0.25～0.3 gram analytical pure Trimethyllaurylammonium bromide being joined volume is to stir in 30 milliliters the mixed solvent of absolute ethyl alcohol and 30 ml deionized water; And then add 0.4～0.8 milliliter of analytical pure tartrate, mix under the normal temperature mixing solutions;
(2) 1～2 milliliter of analytical pure butyl(tetra)titanate is dropwise joined in the mixing solutions that step (1) makes, continue to stir until there not being white floss to occur;
(3) solution that step (2) is made is transferred in 100 milliliters the pyroreaction still;
(4) the pyroreaction still of step (3) is put into thermostatic drying chamber and be incubated 24～48 hours down, naturally cool to room temperature and get white depositions at 120～150 ℃;
(5) white depositions that step (4) is obtained is cleaned 2～3 times with deionized water or absolute ethyl alcohol repeatedly, in loft drier, descends drying promptly to make in 10～12 hours at 60～80 ℃ then and contains three kinds of crystalline phase titanium oxide classification balls.
Cost of the present invention is low, process control procedure is simple, it is extensive synthetic to be prone to, and diameter is arranged is 5～8 microns to the three kinds of crystalline phase titanium oxide classification balls that contain that make, and classification ball surface is by granulometric composition.
Description of drawings
X-ray diffraction (XRD) figure that contains three kinds of crystalline phase titanium oxide classification balls that Fig. 1 makes for the embodiment of the invention 2.
Low power field emission scanning electron microscope (FESEM) figure that contains three kinds of crystalline phase titanium oxide classification balls that Fig. 2 makes for the embodiment of the invention 2.
High power field emission scanning electron microscope (FESEM) figure that contains three kinds of crystalline phase titanium oxide classification balls that Fig. 3 makes for the embodiment of the invention 2.
Embodiment
Embodiment 1:
(1) 0.25 gram analytical pure Trimethyllaurylammonium bromide being joined volume is to stir in 30 milliliters the mixed solvent of absolute ethyl alcohol and 30 ml deionized water; And then add 0.4 milliliter of analytical pure tartrate, mix under the normal temperature mixing solutions;
(2) 1 milliliter of analytical pure butyl(tetra)titanate is dropwise joined in the mixing solutions of step (1), continue to stir until there not being white floss to occur;
(3) solution that step (2) is made is transferred in 100 milliliters the pyroreaction still;
(4) the pyroreaction still of step (3) is put into thermostatic drying chamber and be incubated 24 hours down, naturally cool to room temperature and get white depositions at 120 ℃;
(5) white depositions that step (4) is obtained is with anti-2 times of deionized water or absolute ethyl alcohol, in loft drier, promptly makes in dry 10 hours down at 60 ℃ then and contains three kinds of crystalline phase titanium oxide classification balls.
The three kinds of crystalline phase titanium oxide classification balls that contain that make have good monodispersity, and the classification spherical diameter is about the surface of 6 microns and classification ball by granulometric composition.
Embodiment 2:
(1) 0.3 gram analytical pure Trimethyllaurylammonium bromide being joined volume is to stir in 30 milliliters the mixed solvent of absolute ethyl alcohol and 30 ml deionized water; And then add 0.8 milliliter of analytical pure tartrate, mix under the normal temperature mixing solutions;
(2) 2 milliliters of analytical pure butyl(tetra)titanates are dropwise joined in the mixing solutions of step (1), continue to stir until there not being white floss to occur;
(3) solution that step (2) is made is transferred in 100 milliliters the pyroreaction still;
(4) the pyroreaction still of step (3) is put into thermostatic drying chamber and be incubated 48 hours down, naturally cool to room temperature and get white depositions at 150 ℃;
(5) white depositions that step (4) is obtained is cleaned 3 times with deionized water or absolute ethyl alcohol repeatedly, in loft drier, descends drying promptly to make in 12 hours at 80 ℃ then and contains three kinds of crystalline phase titanium oxide classification balls.
The three kinds of crystalline phase titanium oxide classification balls that contain that make have good monodispersity, and the classification spherical diameter is about the surface of 8 microns and classification ball by granulometric composition.The XRD figure that contains three kinds of crystalline phase titanium oxide classification balls that makes is seen Fig. 1, and the low power FESEM figure that contains three kinds of crystalline phase titanium oxide classification balls that makes sees Fig. 2, and the high power FESEM figure that contains three kinds of crystalline phase titanium oxide classification balls that makes sees Fig. 3.
Claims (1)
1. the preparation method of a titanium oxide classification ball is characterized in that concrete steps are:
(1) 0.25～0.3 gram analytical pure Trimethyllaurylammonium bromide being joined volume is to stir in 30 milliliters the mixed solvent of absolute ethyl alcohol and 30 ml deionized water; And then add 0.4～0.8 milliliter of analytical pure tartrate, mix under the normal temperature mixing solutions;
(2) 1～2 milliliter of analytical pure butyl(tetra)titanate is dropwise joined in the mixing solutions that step (1) makes, continue to stir until there not being white floss to occur;
(3) solution that step (2) is made is transferred in 100 milliliters the pyroreaction still;
(4) the pyroreaction still of step (3) is put into thermostatic drying chamber and be incubated 24～48 hours down, naturally cool to room temperature and get white depositions at 120～150 ℃;
(5) white depositions that step (4) is obtained is cleaned 2～3 times with deionized water or absolute ethyl alcohol repeatedly, in loft drier, promptly makes titanium oxide classification ball down in dry 10～12 hours at 60～80 ℃ then.
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| CN201210022748.2A CN102583526B (en) | 2012-01-31 | 2012-01-31 | Preparation method of titanium dioxide classification balls containing three crystalline phases |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594102A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
| CN101597083A (en) * | 2009-06-29 | 2009-12-09 | 湘潭大学 | A kind of preparation method of monodisperse nano-titanium dioxide |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594102A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
| CN101597083A (en) * | 2009-06-29 | 2009-12-09 | 湘潭大学 | A kind of preparation method of monodisperse nano-titanium dioxide |
Non-Patent Citations (2)
| Title |
|---|
| FRANKLYN, PAUL J等: "Phase transformation of hydrothermally synthesized nanoparticle TiO2: from anatase to rutile nanorods", 《SOUTH AFRICAN JOURNAL OF CHEMISTRY-SUID-AFRIKAANSE TYDSKRIF VIR CHEMIE》, vol. 60, 31 December 2007 (2007-12-31), pages 71 - 75 * |
| KAIFENG YU等: "Preparation of nanosized titanium dioxide from titanium n-butoxide modified with tartaric acid and its influence on the phase transformation", 《MATERIALS LETTERS》, vol. 59, no. 28, 20 July 2005 (2005-07-20), pages 3563 - 3566 * |
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