CN103395831A - Hydrothermal preparation method of shape-controllable titanium dioxide nano tube - Google Patents
Hydrothermal preparation method of shape-controllable titanium dioxide nano tube Download PDFInfo
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Abstract
The invention provides a hydrothermal preparation method of a shape-controllable titanium dioxide nano tube. The hydrothermal preparation method comprises the following steps of: adding 10-50mL of NaOH solution with the concentration being 8-15mol/L into a reaction kettle; then adding 0.1-10g of cetyl trimethyl ammonium bromide and 01-3g of titanium dioxide nano powder into the reaction kettle, and carrying out ultrasonic oscillation to mix the materials uniformly; carrying out hydrothermal reaction in the reaction kettle at the temperature of 100-200 DEG C for 15-30 hours; pouring out supernatant, and washing the obtained solid powder with water to be neutral; adding 0.1-1mol/L of nitric acid or hydrochloric acid into the obtained powder, carrying out ultrasonic oscillation for 1-3 hours at the temperature of 50-100 DEG C; washing a product (which is obtained after acid treatment) with water to be neutral nearly, filtering and drying; and calcining the dried powder for 1-5 hours at the temperature of 400-800 DEG C. The obtained titanium dioxide nano tube is influenced by the adding amount of a surface active agent, the length is controllable, the tube diameter is more uniform, the two ends are open, the tube forming efficiency is high, and therefore the titanium dioxide nano tube can be favorably applied to nanoscience, biomedicine and the like.
Description
Technical field
That the present invention relates to is a kind of preparation method of titania nanotube, is specifically related to a kind of method with the standby controlled titania nanotube powder of pattern of hydro-thermal legal system.
Background technology
Since the people such as Kasuga in 1998 prepared titania nanotube first, this monodimension nanometer material nontoxic, the multiple good characteristic such as chemical stability is high, have air-sensitive, catalytic activity, opto-electronic conversion effect had caused the extensive concern of scientific circles.The preparation method of titania nanotube mainly contains three kinds: hard template method, anonizing and hydrothermal method.Wherein, hydrothermal method is because operating procedure is easy, the titania nanotube purity advantages of higher of preparation has caused scholars' very big interest, a lot of scholar's research the kind of raw material and preparation condition on the impact of nanotube crystal formation, pattern etc. and the formation mechanism of nanotube, but how effectively to control its pattern, prepare the controlled titania nanotube of pattern or a difficult problem.At present, tensio-active agent has been used as soft template and has prepared the nano materials such as nanometer rod, nanoneedle, nanotube, as document " Liu Chao; Zhao Xiujian. surfactant-assisted hydrothermal synthesis TiOx nano pin colloidal sol [J]. Chinese Journal of Inorganic Chemistry; 2007,23 (2): 357-360 " and document " Lv Ruitao, Cao Chuanbao. the preparation of the soft template method of semi-conductor ZnS nanotube with characterize [J]. Science Bulletin; 2004,49 (7): 629-632 ".The method of " titania nanotube " that so far, " efficiently prepares pattern controlled " with tensio-active agent does not also have report.Publication number is in the patent document of CN101239738A, to disclose a kind of preparation method of titania nanotube, and its principal feature is to have prepared the more uniform nanotube of caliber, and unrealized nanotube pattern is controlled.
Summary of the invention
The object of the present invention is to provide a kind of simple to operate, the hydrothermal method preparation method of the controlled titania nanotube of pattern that controllability is strong.
The object of the present invention is achieved like this:
Step 1 is the NaOH solution of 8-15mol/L to adding 10-50mL concentration in reactor;
Step 2, then add 0.1-10g cetyl trimethylammonium bromide, 0.1-3g titanic oxide nano powder in reactor, sonic oscillation makes it to mix;
Step 3, by reactor in 100-200 ℃ of hydro-thermal reaction 15-30h;
Step 4, after hydro-thermal reaction is complete, pour out supernatant liquor, and washing gained pressed powder is to neutral;
Step 5, join the nitric acid of 0.1-1mol/L or hydrochloric acid in the powder of gained 50-100 ℃ of ultrasonic 1-3h;
Step 6, wash the product after acid treatment to approach neutrality;
Step 7, filter;
Step 8, the gained powder is fully dry;
Step 9, calcine 1-5h by dried powder in 400-800 ℃.
Described titanic oxide nano powder is that particle diameter is 10-100nm, and crystal formation is the titanic oxide nano powder of Anatase, Rutile Type or the two mixture.
Although in part background technology document, related to tensio-active agent and be used as soft template and prepare the nano materials such as nanometer rod, nanoneedle, nanotube, method of the present invention and principle are fully different from it.In the present invention, the state of aggregation of tensio-active agent in the environment of concentrated base and High Temperature High Pressure is netted, with very big-difference, the intermediate that netted structure is conducive to react---the stability of titanate nanometer sheet is arranged under mild conditions, and then realize producing of different-shape titania nanotube.
Method provided by the present invention only need be added the tensio-active agent of different amounts in common hydrothermal method process, the conditioned reaction condition, can make the controlled titania nanotube of pattern, and is simple to operate, controllability is strong, can be used for synthesizing in a large number the controlled titania nanotube of pattern.
The present invention adopts tensio-active agent to make soft template and with hydrothermal method, combines and efficiently prepared the controlled titania nanotube of pattern.The gained titania nanotube is subjected to the impact of tensio-active agent addition, and length is controlled, and caliber is more even, and both ends open becomes tube efficiency high, and is very favourable to its application at aspects such as nano science, biomedicines.
The accompanying drawing explanation
Fig. 1 is that common hydrothermal method is the titania nanotube TEM figure of embodiment 1 preparation, and nanotube length is 20-50nm approximately.
Fig. 2 is the prepared titania nanotube TEM figure of embodiment 2, and nanotube length is 50-100nm approximately.
Fig. 3 is the prepared titania nanotube TEM figure of embodiment 3, and nanotube length is the hundreds of nanometer.
Embodiment
Below for example the present invention is done to more detailed description.
Embodiment 1:
Step 1, configuration 20mL concentration are that the NaOH solution of 10mol/L adds in reactor.
Step 2, weighing 3g particle diameter is the anatase phase titanium dioxide nanometer powder of 15nm, adds sonic oscillation in the concentrated alkali solution for preparing to make it to mix.
Step 3, put into baking oven in 130 ℃ of hydro-thermal reaction 30h by reactor.
Step 4, after hydro-thermal reaction is complete, pour out supernatant liquor, and washing gained pressed powder is to neutral.
Step 5, join the nitric acid of 0.1mol/L or hydrochloric acid in the powder of gained 50-100 ℃ of ultrasonic 1-3h.
Step 6, wash the sample after acid treatment to approach neutrality.
Step 7, filter.
Step 8, the gained powder is fully dry.
Step 9, calcine 2h by dried powder in 400 ℃.
Embodiment 2:
Step 1, configuration 20mL concentration are that the NaOH solution of 10mol/L adds in reactor.
Step 2, weighing 0.05g cetyl trimethylammonium bromide, 3g particle diameter are the anatase phase titanium dioxide nanometer powder of 15nm, add sonic oscillation in the concentrated alkali solution for preparing to make it to mix.
Step 3, put into baking oven in 130 ℃ of hydro-thermal reaction 30h by reactor.
Step 4, after hydro-thermal reaction is complete, pour out supernatant liquor, and washing gained pressed powder is to neutral.
Step 5, join the nitric acid of 0.1mol/L or hydrochloric acid in the powder of gained 50-100 ℃ of ultrasonic 1-3h.
Step 6, wash the sample after acid treatment to approach neutrality.
Step 7, filter.
Step 8, the gained powder is fully dry.
Step 9, calcine 2h by dried powder in 400 ℃.
Embodiment 3:
Step 1, configuration 20mL concentration are that the NaOH solution of 10mol/L adds in reactor.
Step 2, weighing 0.1g cetyl trimethylammonium bromide, 3g particle diameter are the anatase phase titanium dioxide nanometer powder of 15nm, add sonic oscillation in the concentrated alkali solution for preparing to make it to mix.
Step 3, put into baking oven in 130 ℃ of hydro-thermal reaction 30h by reactor.
Step 4, after hydro-thermal reaction is complete, pour out supernatant liquor, and washing gained pressed powder is to neutral.
Step 5, join the nitric acid of 0.1mol/L or hydrochloric acid in the powder of gained 50-100 ℃ of ultrasonic 1-3h.
Step 6, wash the sample after acid treatment to approach neutrality.
Step 7, filter.
Step 8, the gained powder is fully dry.
Step 9, calcine 2h by dried powder in 400 ℃.
Claims (2)
1. the hydrothermal method preparation method of the controlled titania nanotube of pattern is characterized in that:
Step 1 is the NaOH solution of 8-15mol/L to adding 10-50mL concentration in reactor;
Step 2, then add 0.1-10g cetyl trimethylammonium bromide, 0.1-3g titanic oxide nano powder in reactor, sonic oscillation makes it to mix;
Step 3, by reactor in 100-200 ℃ of hydro-thermal reaction 15-30h;
Step 4, after hydro-thermal reaction is complete, pour out supernatant liquor, and washing gained pressed powder is to neutral;
Step 5, join the nitric acid of 0.1-1mol/L or hydrochloric acid in the powder of gained 50-100 ℃ of ultrasonic 1-3h;
Step 6, wash the product after acid treatment to approach neutrality;
Step 7, filter;
Step 8, the gained powder is fully dry;
Step 9, calcine 1-5h by dried powder in 400-800 ℃.
2. the hydrothermal method preparation method of the controlled titania nanotube of pattern according to claim 1, it is characterized in that: described titanic oxide nano powder is that particle diameter is 10-100nm, and crystal formation is the titanic oxide nano powder of Anatase, Rutile Type or the two mixture.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105080529A (en) * | 2014-05-13 | 2015-11-25 | 江苏瑞丰科技实业有限公司 | Normal temperature catalytic material for efficiently removing VOCs |
| CN107349944A (en) * | 2017-08-31 | 2017-11-17 | 桂林融通科技有限公司 | A kind of preparation method of silver bromide titanium dioxide nano-tube composite catalyst |
| CN109174051A (en) * | 2018-08-28 | 2019-01-11 | 武汉理工大学 | A kind of preparation method protonating titanate nanotube and its adsorption applications to uranium, caesium |
| CN115073387A (en) * | 2022-07-14 | 2022-09-20 | 绍兴迪飞新材料有限公司 | Preparation method of electrically polarized particles and application of electrically polarized particles to electrically polarized color-changing optical film |
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| CN1528672A (en) * | 2003-09-26 | 2004-09-15 | 清华大学 | Titanium oxide nano tube and preparing method thereof |
| CN101468812A (en) * | 2007-12-24 | 2009-07-01 | 比亚迪股份有限公司 | Preparation of titanium dioxide nano-rod |
| CN103084157A (en) * | 2013-01-29 | 2013-05-08 | 山东轻工业学院 | Large-tube-diameter TiO2 nano tube and synthesizing method thereof as well as application of nano tube in photocatalytic degradation of papermaking wastewater |
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2013
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| CN1528672A (en) * | 2003-09-26 | 2004-09-15 | 清华大学 | Titanium oxide nano tube and preparing method thereof |
| CN101468812A (en) * | 2007-12-24 | 2009-07-01 | 比亚迪股份有限公司 | Preparation of titanium dioxide nano-rod |
| CN103084157A (en) * | 2013-01-29 | 2013-05-08 | 山东轻工业学院 | Large-tube-diameter TiO2 nano tube and synthesizing method thereof as well as application of nano tube in photocatalytic degradation of papermaking wastewater |
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| CHIEN-CHENG TSAI ET AL.: "Structural Features of Nanotubes Synthesized from NaOH Treatment on TiO2 with Different Post-Treatments", 《CHEM. MATER.》 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105080529A (en) * | 2014-05-13 | 2015-11-25 | 江苏瑞丰科技实业有限公司 | Normal temperature catalytic material for efficiently removing VOCs |
| CN105080529B (en) * | 2014-05-13 | 2017-12-29 | 江苏瑞丰科技实业有限公司 | Normal-temperature efficient removes VOCs catalysis materials |
| CN107349944A (en) * | 2017-08-31 | 2017-11-17 | 桂林融通科技有限公司 | A kind of preparation method of silver bromide titanium dioxide nano-tube composite catalyst |
| CN109174051A (en) * | 2018-08-28 | 2019-01-11 | 武汉理工大学 | A kind of preparation method protonating titanate nanotube and its adsorption applications to uranium, caesium |
| CN115073387A (en) * | 2022-07-14 | 2022-09-20 | 绍兴迪飞新材料有限公司 | Preparation method of electrically polarized particles and application of electrically polarized particles to electrically polarized color-changing optical film |
| CN115073387B (en) * | 2022-07-14 | 2023-08-11 | 绍兴迪飞新材料有限公司 | Preparation method of electrically polarized particles and application of electrically polarized particles in electrically polarized color-changing optical film |
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Application publication date: 20131120 |