CN101580276A - Preparation method of highly dispersive spindle-shaped nano titanium dioxide sol - Google Patents
Preparation method of highly dispersive spindle-shaped nano titanium dioxide sol Download PDFInfo
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- CN101580276A CN101580276A CNA2009100404004A CN200910040400A CN101580276A CN 101580276 A CN101580276 A CN 101580276A CN A2009100404004 A CNA2009100404004 A CN A2009100404004A CN 200910040400 A CN200910040400 A CN 200910040400A CN 101580276 A CN101580276 A CN 101580276A
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Abstract
The invention provides a preparation method of highly dispersive spindle-shaped nano titanium dioxide sol. The method comprises the following steps: adding ammonia with mass concentration being 10%-50% into aqueous solution containing titanyl sulfate, adjusting pH value to be 7.5-11; stirring and reacting for over 4 hours to obtain white precipitation, washing by deionized water and centrifugating for several times; mixing the white precipitation with the deionized water, adjusting pH value to be 1-7, stirring for over 2 hours to obtain highly dispersive spindle-shaped nano titanium dioxide sol. The invention improves traditional low-temperature synthesis technology, and the dispersibility of the prepared product is greatly improved; the spindle-shaped nano titanium dioxide has better biocompatibility and good biological security, and the invention has simple preparation method and low cost and is beneficial for industrialized production.
Description
Technical field
The present invention relates to the preparing technical field of TiO 2 sol, be specifically related to the preparation method of highly dispersive spindle-shaped nano titanium dioxide.
Background technology
In all semiconductor light-catalysts,, thereby be considered to have application potential most because titanium dioxide has strong, the synthetic low cost and other advantages of good biological and chemical inertia, strong oxidizing property, anti-photoetch and chemical corrosion ability.Find first that from Frank and Bark in 1997 titanium dioxide can be used for having had increasing scientist to be engaged in about titanium dioxide in the applied research aspect the environment protection since the prussiate in the degradation of sewage.Particularly at aspects such as the purifying of water, purifying air, antibiotic and sterilizing, cancer therapy, sewage disposals.
The method of synthesis of nano titanium dioxide is a lot,, magnetron sputtering synthetic as sol-gel method, chemical precipitation method, hydro-thermal etc.But, sol-gel method enjoys favor owing to having numerous advantages such as simple such as preparation technology, that product purity is high, particle size is little, but blemish in an otherwise perfect thing is the agglomeration traits that be difficult to solve preparation process, thereby makes quantum yield reduce greatly and cause organic pollutant degradation efficiency to descend suddenly.In order to address the above problem, in recent years, the countries in the world scientist has expected various ways.Such as particle surface organic chelated (K.T.Ranjit etc., J.Phys.Chem.B.1998.102.9397-9403); Nonmetal doping (S.Yin etc., J Mater Sci, 2008.43.2240-2246; V.Balek etc., J.Therm.Spray.Technol, 2008.92.161-167); Transient metal doped (X.Z.Li etc., Environ.Sci.Technol, 2001.35.2381-2387; A.D.Paola etc., J.Phys.Chem.B, 2002.106.637-645); Semi-conductor coupling (R.Vogel etc., J Phys Chem, 1994.98.3183-3188; D.W.Kim etc., Int.J.Hydrogen.Energy, 2007.32.3137-3140); Dye sensitization (J.G.Yu etc., J.Solid.State Chem, 2003.174.372-380).These methods all can improve quantum yield in various degree, but consider preparation technology, synthetic cost and test conditions, and these also are not ideal methods comparatively.
Simultaneously, along with the fast development of nanosecond science and technology, nano material and people's life is more and more closer.Therefore it is particularly important to consider that the security of prepared material becomes.Yet few in number studies show that, such as Single Walled Carbon Nanotube, polytetrafluorethylenano nano particle overt toxicity (J.L.Mauderly etc., J.Res.Rep.Health.Eff.Inst, 1994.68.1-75 is arranged all; A.Shvedova etc., J.Toxicol.Environ.Health A, 2003.66.1909-1926; G.Oberdorster etc., Res.Rep.Health.Eff.Inst, 2000.96.5-74).Therefore, be in security consideration, the introducing of nonmetal, transition metal, dyestuff, organism etc. all might bring unsafe factor.
In view of the above-mentioned variety of problems of mentioning, we have synthesized high purity, high dispersive, avirulent nano titanic oxide sol by improving the technology of traditional cryosol gel method.It has good stability, and has broad application prospects.
Summary of the invention
The objective of the invention is to overcome the prior art above shortcomings, the preparation method of highly dispersive spindle-shaped nano titanium dioxide sol is provided.This method adopts traditional low temperature synthetic technology, and synthesis technique is simple, is easy to industrialization.Concrete technical scheme is as follows:
The preparation method of highly dispersive spindle-shaped nano titanium dioxide sol comprises the steps:
(1) titanyl sulfate being dissolved in deionized water, is 7.5～11 by adding ammoniacal liquor adjusting pH value then;
(2) stirring reaction gets white precipitate, with deionized water wash and centrifugal;
(3) white precipitate is mixed with deionized water, regulating pH value under agitation condition is 1～7, obtains highly dispersive spindle-shaped nano titanium dioxide sol again.
Among the above-mentioned preparation method, the mass concentration of the described ammoniacal liquor of step (1) is 10%～50%.
Among the above-mentioned preparation method, step (2) is described to be 4 times with deionized water wash and centrifugal number of times.
Among the above-mentioned preparation method, the described stirring reaction of step (2) is at room temperature carrying out.The rotating speed that described stirring is adopted is 500～800 rev/mins.The rotating speed of described centrifugal employing is 5000～8000 rev/mins.
Among the above-mentioned preparation method, the diameter of described highly dispersive spindle-shaped nano titanium dioxide sol is 20-25nm, and long is 40-50nm, and is anatase crystal.
Among the above-mentioned preparation method, step (3) is 1～7 by dripping hydrogen peroxide adjusting pH value.
Among the above-mentioned preparation method, the time of the described stirring reaction of step (2) is more than 4 hours.The time length of the described stirring of step (3) is more than 2 hours.
The present invention adopts improved traditional low temperature titanyl sulfate method for hydrolysis to obtain the nano titanic oxide sol of high dispersive.Its particle becomes fusiformis, and diameter is about 25nm, is about to be to be anatase crystal by 50nm.In fields such as Industrial Catalysis, sewage disposal, purifying air, disinfection, cancer therapy very big application potential is arranged.
The present invention has following characteristics:
1, improves traditional low temperature synthesis technique, do not need water bath with thermostatic control heat-processed, find out that by transmission electron microscope photo its product has very high dispersiveness, used medicine such as titanyl sulfate, ammoniacal liquor are all originated abundant, with low cost, only need twice adjust pH process, synthesis technique is simple, helps suitability for industrialized production.
2, by the toxicity of this nano titanium oxide of research, find that this product does not produce overt toxicity to this cell to mouse entocuticle cell.
Description of drawings
Fig. 1 is the nano titanic oxide sol transmission electron microscope figure for preparing in the embodiment, and its particle high dispersing is fusiformis.
Fig. 2 is the x-ray diffraction pattern of nano titanium oxide xerogel shown in Figure 1, and its crystal formation is a Detitanium-ore-type.
Fig. 3 is the Fourier transform infrared spectroscopy figure of nano titanium oxide xerogel shown in Figure 1.
Fig. 4 is the variation diagram of mouse endothelial cell activity with the nano titanium oxide concentration of this programme preparation, when finding out that by figure even titanium dioxide concentration reaches 250 μ g/ml, the activity of mouse endotheliocyte illustrates that still more than 80% the nano titanic oxide sol of this method preparation has better biocompatibility and good biological safety.
Embodiment
Following embodiment further specifies of the present invention, and the present invention need not to limit the magnitude relation of using between titanyl sulfate and the deionized water, is dissolved in deionized water as long as satisfy titanyl sulfate, and following examples are not limitations of the present invention.
Embodiment 1
Taking by weighing the 3g titanyl sulfate and be dissolved in the 500ml deionized water, stir with 800 speed of changeing per minutes at ambient temperature, is that 10% ammoniacal liquor dropwise adds wherein to the pH value and equals 7.5 with mass concentration.Continue to stir after 4 hours, the white precipitate that generates with deionized water wash, and be centrifugal 4 times of 8000 speed with rotating speed.Centrifugal product with after the 600ml deionized water mixes, is at the uniform velocity stirred with 400 speed of changeing per minutes, drip hydrogen peroxide and regulate pH value to 1, continue again to stir and obtained highly dispersive spindle-shaped nano titanium dioxide sol in 6 hours.As Fig. 1, the fusiformis particle of the high dispersive of TEM photo clear display, diameter is about 25nm, long is about 50nm; As Fig. 2, xerogel XRD figure spectrum is corresponding with the JCPDS card that is numbered 73-1764, illustrates that its crystal formation is an anatase octahedrite; Fig. 3 is the Fourier transform infrared spectroscopy figure of nano titanium oxide xerogel, and infared spectrum has tangible absorption band at the 1630cm-1 place, illustrates that this colloidal sol contains a large amount of titanium hydroxyls; When the TiO 2 sol that adopts 250 μ g/mL was handled the mouse endotheliocyte, its cytoactive was still high to 81.5% (as Fig. 4), and not toxigenicity of the contained nano particle pair cell of this colloidal sol is described.
Embodiment 2
Taking by weighing the 1g titanyl sulfate and be dissolved in the 200ml deionized water, stir with 600 speed of changeing per minutes at ambient temperature, is that 30% ammoniacal liquor dropwise adds wherein to the pH value and equals 11 with mass concentration.Continue to stir after 6 hours, the white precipitate that generates with deionized water wash, and be centrifugal 4 times of 5000 speed with rotating speed.Centrifugal product with after the 400ml deionized water mixes, is at the uniform velocity stirred with 400 speed of changeing per minutes, drip hydrogen peroxide and regulate pH value to 5, continue again to stir and obtained highly dispersive spindle-shaped nano titanium dioxide sol in 5 hours.Xerogel XRD figure spectrum shows that its crystal formation is an anatase octahedrite, and the demonstration of TEM photo disperses fusiformis particle preferably, and diameter is about 20nm, is about to be 40nm.
Embodiment 3
Taking by weighing the 5g titanyl sulfate and be dissolved in the 500ml deionized water, stir with 500 speed of changeing per minutes at ambient temperature, is that 50% ammoniacal liquor dropwise adds wherein to the pH value and equals 8 with mass concentration.Continue to stir after 8 hours, the white precipitate that generates with deionized water wash, and be centrifugal 4 times of 6000 speed with rotating speed.Centrifugal product with after the 300ml deionized water mixes, is at the uniform velocity stirred with 400 speed of changeing per minutes, regulate pH value to 6, continue again to stir and obtained highly dispersive spindle-shaped nano titanium dioxide sol in 4 hours.Xerogel XRD figure spectrum shows that its crystal formation is an anatase octahedrite, and the fusiformis particle of the high dispersive of TEM photo clear display, diameter are 25nm, and long is 50nm.
Embodiment 4
Taking by weighing the 4g titanyl sulfate and be dissolved in the 700ml deionized water, stir with 600 speed of changeing per minutes at ambient temperature, is that 20% ammoniacal liquor dropwise adds wherein to the pH value and equals 10 with mass concentration.Continue to stir after 10 hours, the white precipitate that generates with deionized water wash, and be centrifugal 4 times of 7000 speed with rotating speed.Centrifugal product with after the 400ml deionized water mixes, and is at the uniform velocity stirred with 400 speed of changeing per minutes, regulate pH value to 7, continue again to stir and obtained disperseing fusiformis nano titanic oxide sol preferably in 2 hours.Xerogel XRD figure spectrum shows that its crystal formation is an anatase octahedrite, and the dispersion of TEM photo clear display is the fusiformis particle preferably, and diameter is 20nm, is about to be 45nm.
Claims (10)
1, the preparation method of highly dispersive spindle-shaped nano titanium dioxide sol is characterized in that comprising the steps:
(1) titanyl sulfate being dissolved in deionized water, is 7.5～11 by adding ammoniacal liquor adjusting pH value then;
(2) stirring reaction gets white precipitate, with deionized water wash and centrifugal;
(3) white precipitate is mixed with deionized water, regulating pH value under agitation condition is 1～7, obtains highly dispersive spindle-shaped nano titanium dioxide sol again.
2, preparation method according to claim 1 is characterized in that the mass concentration of the described ammoniacal liquor of step (1) is 10%～50%.
3, preparation method according to claim 1, it is characterized in that step (2) described be 4 times with deionized water wash and centrifugal number of times.
4, preparation method according to claim 1 is characterized in that the described stirring reaction of step (2) at room temperature carries out.
5, preparation method according to claim 1 is characterized in that the rotating speed that described stirring is adopted is 500～800 rev/mins.
6, preparation method according to claim 1, the rotating speed that it is characterized in that described centrifugal employing is 5000～8000 rev/mins.
7, preparation method according to claim 1, the diameter that it is characterized in that described highly dispersive spindle-shaped nano titanium dioxide sol is 20-25nm, long is 40-50nm, and is anatase crystal.
8, preparation method according to claim 1 is characterized in that step (3) is 1～7 by dripping hydrogen peroxide adjusting pH value.
9,, it is characterized in that the time of the described stirring reaction of step (2) is more than 4 hours according to each described preparation method of claim 1～8.
10,, it is characterized in that the time length of the described stirring of step (3) is more than 2 hours according to each described preparation method of claim 1～8.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295310A (en) * | 2010-06-28 | 2011-12-28 | 中国科学院理化技术研究所 | Preparation method of metal-ion-doped titanium dioxide transparent aqueous sol |
| CN102560649A (en) * | 2012-01-12 | 2012-07-11 | 中国科学院合肥物质科学研究院 | Flowerlike-structure titanium dioxide formed by spindle single crystal and preparation method thereof |
| CN102786087A (en) * | 2012-08-22 | 2012-11-21 | 厦门大学 | Method for preparing titanium dioxide sol |
| CN103848458A (en) * | 2012-11-29 | 2014-06-11 | 中国科学院合肥物质科学研究院 | Nitrogen-doped rutile crystal-type titanium dioxide nano-rods and preparation method thereof |
| CN105417575A (en) * | 2015-12-14 | 2016-03-23 | 上海交通大学 | Preparation method of monodisperse tin dioxide quantum dot hydrosol |
| CN106824152A (en) * | 2017-03-23 | 2017-06-13 | 重庆交通大学 | A kind of TiO 2 sol and preparation method thereof |
| CN106890656A (en) * | 2017-03-23 | 2017-06-27 | 重庆交通大学 | A kind of phosphorus doping TiO 2 sol and preparation method thereof |
| CN112357954A (en) * | 2020-11-13 | 2021-02-12 | 中国科学院合肥物质科学研究院 | Shuttle structure H2Ti5O11·H2Solvothermal synthesis method of O nano material and application of lithium battery electrode material |
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2009
- 2009-06-19 CN CNA2009100404004A patent/CN101580276A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295310A (en) * | 2010-06-28 | 2011-12-28 | 中国科学院理化技术研究所 | Preparation method of metal-ion-doped titanium dioxide transparent aqueous sol |
| CN102560649A (en) * | 2012-01-12 | 2012-07-11 | 中国科学院合肥物质科学研究院 | Flowerlike-structure titanium dioxide formed by spindle single crystal and preparation method thereof |
| CN102560649B (en) * | 2012-01-12 | 2014-07-30 | 中国科学院合肥物质科学研究院 | Flowerlike-structure titanium dioxide formed by spindle single crystal and preparation method thereof |
| CN102786087A (en) * | 2012-08-22 | 2012-11-21 | 厦门大学 | Method for preparing titanium dioxide sol |
| CN103848458A (en) * | 2012-11-29 | 2014-06-11 | 中国科学院合肥物质科学研究院 | Nitrogen-doped rutile crystal-type titanium dioxide nano-rods and preparation method thereof |
| CN105417575A (en) * | 2015-12-14 | 2016-03-23 | 上海交通大学 | Preparation method of monodisperse tin dioxide quantum dot hydrosol |
| CN105417575B (en) * | 2015-12-14 | 2017-05-31 | 上海交通大学 | A kind of preparation method of the single dispersing tin dioxide quantal-point hydrosol |
| CN106824152A (en) * | 2017-03-23 | 2017-06-13 | 重庆交通大学 | A kind of TiO 2 sol and preparation method thereof |
| CN106890656A (en) * | 2017-03-23 | 2017-06-27 | 重庆交通大学 | A kind of phosphorus doping TiO 2 sol and preparation method thereof |
| CN112357954A (en) * | 2020-11-13 | 2021-02-12 | 中国科学院合肥物质科学研究院 | Shuttle structure H2Ti5O11·H2Solvothermal synthesis method of O nano material and application of lithium battery electrode material |
| CN112357954B (en) * | 2020-11-13 | 2022-08-05 | 中国科学院合肥物质科学研究院 | Shuttle structure H 2 Ti 5 O 11 ·H 2 Solvothermal synthesis method of O nano material and application of lithium battery electrode material |
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Open date: 20091118 |