CN101172650A - Method for controlling nano-anatase TiO* feature with NaAc as additive agent - Google Patents
Method for controlling nano-anatase TiO* feature with NaAc as additive agent Download PDFInfo
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- CN101172650A CN101172650A CNA2007100472765A CN200710047276A CN101172650A CN 101172650 A CN101172650 A CN 101172650A CN A2007100472765 A CNA2007100472765 A CN A2007100472765A CN 200710047276 A CN200710047276 A CN 200710047276A CN 101172650 A CN101172650 A CN 101172650A
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- anatase tio
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Abstract
The invention relates to a method for controlling the appearance of the anatase Tio2 by taking NaAc as additive. The method comprises the steps as follow: (1) isopropyl titanate is used as the raw material and trolamine is used as stabilizing agent, and then water is added into to form the Ti4+ solution, and the mol rate of trolamine and isopropyl titanate is 0: 1.0; (2) water is added into the Ti4+ solution in the same volume of the Ti4+ solution and then is mixed evenly; (3) the additive NaAc which is used for controlling the appearance is added into, and the solution PH value is adjusted to implement a first aging so as to obtain viscolloid; and (4) the nanometer anatase Tio2 grain is obtained after being aged by gelling. The anatase TiO2 prepared with the invention has the advantages of even granularity, good dispersivity, simple preparation technology and easy generalization, thereby being capable of controlling the appearance into a cube shape and a stick shape.
Description
Technical field
The invention belongs to the nano-titanium dioxide powder field, particularly relating to a kind of is additive control nano-anatase TiO with NaAc
2The method of pattern.
Background technology
Nearest studies show that not only the size and the size of nano material can influence its performance, and also there is remarkably influenced in its pattern to its various performances.Present research is more to be concentrated on by changing different technologies of preparing, obtains difform nano particle as sol-gel method, hydrothermal method, vapor phase process with expectation.And the employing additive is as less the appearing in the newspapers of research document of nano material style control agent.
Nano-titanium dioxide powder is a kind of novel inorganic materials, because of its particle diameter little, specific surface area is big, photochemical catalysis, absorption ultraviolet ray ability are strong, and nontoxic, advantages such as catalytic activity is high, good stability get more and more people's extensive concerning, and being considered to has wide application prospect at aspects such as solar energy converting and utilization, environmental purification.Wherein titanium dioxide has anatase octahedrite, rutile and three kinds of mineral of brookite, and is wherein best with the photochemical activity of anatase octahedrite.Difform in recent years TiO
2Nano particle is produced out, as nanometer rod, and (Solid State Chem.2004 such as nano wire, nanotube, nanometer sheet; 32:33).And with additive as TiO
2The rare bibliographical information of the research of nano particle style control agent.People such as Sugimoto have reported with primary amine, swollen amine, tertiary amine as nano-TiO
2The research of particle shape control agent, they find can control TiO by suitably controlling reaction conditions
2Particle changes (J.Colloid Interf.Sci.2003 by cube to ellipse; 259 53).And with NaAc as additive, control nano-anatase TiO
2The research of pattern yet there are no bibliographical information.
Summary of the invention
The purpose of this invention is to provide a kind of is additive control nano-anatase TiO with NaAc
2The method of pattern, this method are to be presoma with the stable titanium isopropylate of trolamine, and adopting NaAc is the nano particle style control agent, the anatase octahedrite TiO for preparing
2Granule-morphology is controlled to be made as cubicly and bar-shaped, and technology and equipment are simple, constant product quality, and good reproducibility.
Of the present invention is additive control nano-anatase TiO with NaAc
2The method of pattern comprises the following steps:
(1) be raw material with the titanium isopropylate, trolamine is a stablizer, adds water, forms Ti
4+Solution, trolamine and titanium isopropylate molar weight are than being 0-1.0;
(2) Ti
4+Add water in the solution, stir with volume;
(3) add morphology control additive NaAc, regulator solution pH value is carried out the ageing first time, gets viscoloid;
(4) gel carries out the ageing second time, gets nano-anatase TiO
2Particle.
Described NaAc is a 0.2-1.0mol/L NaAc solution, preferred 0.2-0.5mol/L;
PH value in the described step (3) is between 0-11, and pH value regulator solution is perchloric acid or sodium hydroxide solution;
The described ageing first time is that solution places hydrothermal reaction kettle in 80-120 ℃ of following ageing 12-36 hour;
The described ageing second time be sample in hydrothermal reaction kettle at 100-160 ℃ of ageing 24-48 hour.
Described nano-anatase TiO
2Particle is cube nano-anatase TiO
2Particle or rod-like nano anatase octahedrite TiO
2Particle.
The nano-anatase TiO that method of the present invention is prepared
2, epigranular, good dispersity, pattern may be controlled to cubic and bar-shaped, and preparation technology is simple, are convenient to promote.
Description of drawings
Fig. 1 is a main technique schema of the present invention;
Fig. 2 is the nano-anatase TiO that the method that provides among the embodiment of the invention 1-3 is prepared
2XRD (X-ray diffraction, X-ray diffraction) analyze;
Fig. 3 is the nano-anatase TiO that method provided by the invention is prepared under pH value 9.5, different concns NaAc
2The transmission electron microscope picture of powder (a) is the transmission electron microscope picture of embodiment 1, and (c) transmission electron microscope picture of embodiment 2 (d) is the transmission electron microscope picture of embodiment 3;
Fig. 4 is that method provided by the invention is the nano-anatase TiO for preparing under the different pH values of 0.5mol/l in NaAc concentration
2The transmission electron microscope picture of powder (a) is the transmission electron microscope picture of embodiment 4, (b) is the transmission electron microscope picture of embodiment 5, (c) is the transmission electron microscope picture of embodiment 6.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
A) take by weighing the titanium isopropylate of 0.02mol, add the trolamine of 0.01mol, add the Ti that deionized water is mixed with 0.5mol/l
4+Solution;
B) get 10ml step a) solution and mix with the volume deionized water;
C) with b) gained solution is adjusted to pH value 9.5 with NaOH solution, ageing 24h next time in 100 ℃ of hydrothermal reaction kettles;
D) with the ageing 72 hours in 140 ℃ of hydrothermal reaction kettles of the viscoloid of step c).
The nano-anatase TiO of present method preparation
2XRD (X-ray diffraction, X-ray diffraction) analyze and to see that accompanying drawing 2, its transmission electron microscope picture see accompanying drawing 3 (a), particle diameter is 21 nanometers.
A) take by weighing the titanium isopropylate of 0.02moL, add the trolamine of 0.01moL, add the Ti that deionized water is mixed with 0.5moL/L
4+Solution;
B) sodium acetate soln of preparation 0.5moL/L;
C) get 10mL step a) solution and mix, get 10mL b with the volume deionized water) the solution uniform mixing;
D) with c) gained solution is adjusted to pH value 9.5 with NaOH solution, ageing 24h in 100 ℃ of hydrothermal reaction kettles;
E) with the ageing 96 hours in 130 ℃ of hydrothermal reaction kettles of the viscoloid of step d).
The nano-anatase TiO of present method preparation
2XRD analysis see accompanying drawing 2, its transmission electron microscope picture is seen accompanying drawing 3 (c), particle diameter is 20.2 * 38.0 nanometers.
A) take by weighing the titanium isopropylate of 0.02moL, add the trolamine of 0.01moL, add the Ti that deionized water is mixed with 0.5moL/L
4+Solution;
B) sodium acetate soln of preparation 1.0moL/L;
C) get 10mL step a) solution and mix, get 10mL b with the volume deionized water) the solution uniform mixing;
D) with c) gained solution is adjusted to pH value 9.5 with NaOH solution, in 110 ℃ of ageing 36h next time;
E) with the viscoloid of step d) in 120 ℃ of ageings 96 hours.
The nano-anatase TiO of present method preparation
2XRD analysis see accompanying drawing 2, its transmission electron microscope picture is seen accompanying drawing 3 (d), particle diameter is 23.1 * 48.4 nanometers.
Embodiment 4
A) take by weighing the titanium isopropylate of 0.02moL, add the trolamine of 0.01moL, add the Ti that deionized water is mixed with 0.5moL/L
4+Solution;
B) sodium acetate soln of preparation 1.0moL/L;
C) get 10mL step a) solution and mix, get 10mLb with the volume deionized water) the solution uniform mixing;
D) with c) gained solution HCLO
4Solution is adjusted to pH value 0.9, in 110 ℃ of ageing 36h next time;
E) with the viscoloid of step d) in 120 ℃ of ageing 96h;
The nano-anatase TiO of present method preparation
2XRD analysis see accompanying drawing 2, its transmission electron microscope picture is seen accompanying drawing 4 (a), particle diameter is 14.1 nanometers.
Embodiment 5
A) take by weighing the titanium isopropylate of 0.02moL, add the trolamine of 0.01moL, add the Ti that deionized water is mixed with 0.5moL/L
4+Solution;
B) sodium acetate soln of preparation 1.0moL/L.
F) get 10mL step a) solution and mix, get 10mLb with the volume deionized water) the solution uniform mixing.
G) with c) gained solution HCLO
4Solution is adjusted to pH value 4.3, in 110 ℃ of ageing 36h next time;
The nano-anatase TiO of present method preparation
2Transmission electron microscope picture see accompanying drawing 4 (b), particle diameter is 19.2 nanometers.
Embodiment 6
A) take by weighing the titanium isopropylate of 0.02moL, add the trolamine of 0.01moL, add the Ti that deionized water is mixed with 0.5moL/L
4+Solution;
B) sodium acetate soln of preparation 1.0moL/L;
C) get 10mL step a) solution and mix, get 10mLb with the volume deionized water) solution evenly mixes;
D) with c) gained solution is adjusted to pH value 7.9 with NaOH solution, in 110 ℃ of ageing 36h next time;
E) with the viscoloid of step d) in 120 ℃ of ageing 96h.
The nano-anatase TiO of present method preparation
2Transmission electron microscope picture see accompanying drawing 4 (c), particle diameter is 20.3 nanometers.
Claims (7)
1. with NaAc additive control nano-anatase TiO
2The method of pattern comprises the following steps:
(1) be raw material with the titanium isopropylate, trolamine is a stablizer, adds water, forms Ti
4+Solution, trolamine and titanium isopropylate molar weight are than being 0-1.0;
(2) Ti
4+Add water in the solution, stir with volume;
(3) add morphology control additive NaAc, regulator solution pH value is carried out the ageing first time, gets viscoloid;
(4) gel carries out the ageing second time, gets nano-anatase TiO
2Particle.
2. according to claim 1 is additive control nano-anatase TiO with NaAc
2The method of pattern is characterized in that: described NaAc is a 0.2-1.0mol/LNaAc solution.
3. according to claim 2 is additive control nano-anatase TiO with NaAc
2The method of pattern is characterized in that: described NaAc is a 0.2-0.5mol/L NaAc solution.
4. according to claim 1 is additive control nano-anatase TiO with NaAc
2The method of pattern is characterized in that: the pH value in the described step (3) is between 0-11, and pH value regulator solution is perchloric acid or sodium hydroxide solution.
5. according to claim 1 is additive control nano-anatase TiO with NaAc
2The method of pattern is characterized in that: the described ageing first time is that solution places hydrothermal reaction kettle in 80-120 ℃ of following ageing 12-36 hour.
6. according to claim 1 is additive control nano-anatase TiO with NaAc
2The method of pattern is characterized in that: the described ageing second time be sample in hydrothermal reaction kettle at 100-160 ℃ of ageing 24-48 hour.
7. according to claim 1 is additive control nano-anatase TiO with NaAc
2The method of pattern is characterized in that: described nano-anatase TiO
2Particle is cube nano-anatase TiO
2Particle or rod-like nano anatase octahedrite TiO
2Particle.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880057A (en) * | 2010-06-04 | 2010-11-10 | 山东轻工业学院 | Method for preparing high-purity brookite titanium dioxide with controlled appearance |
| CN102602989A (en) * | 2012-03-21 | 2012-07-25 | 奇瑞汽车股份有限公司 | Titanium dioxide as well as preparation method thereof, slurry material of solar battery as well as preparation method thereof and solar battery |
| CN103700503A (en) * | 2013-12-30 | 2014-04-02 | 中国科学院上海硅酸盐研究所 | Method for preparing shape-controllable dye-sensitized solar cell photo-anode |
| 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 |
-
2007
- 2007-10-19 CN CNB2007100472765A patent/CN100567166C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880057A (en) * | 2010-06-04 | 2010-11-10 | 山东轻工业学院 | Method for preparing high-purity brookite titanium dioxide with controlled appearance |
| CN102602989A (en) * | 2012-03-21 | 2012-07-25 | 奇瑞汽车股份有限公司 | Titanium dioxide as well as preparation method thereof, slurry material of solar battery as well as preparation method thereof and solar battery |
| CN103700503A (en) * | 2013-12-30 | 2014-04-02 | 中国科学院上海硅酸盐研究所 | Method for preparing shape-controllable dye-sensitized solar cell photo-anode |
| CN103700503B (en) * | 2013-12-30 | 2017-02-08 | 中国科学院上海硅酸盐研究所 | Method for preparing shape-controllable dye-sensitized solar cell photo-anode |
| 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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| CN100567166C (en) | 2009-12-09 |
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Granted publication date: 20091209 Termination date: 20121019 |