CN103288126A - Method of preparing titanium dioxide nanotube with assistance of cationic surface active agent - Google Patents
Method of preparing titanium dioxide nanotube with assistance of cationic surface active agent Download PDFInfo
- Publication number
- CN103288126A CN103288126A CN2013101772832A CN201310177283A CN103288126A CN 103288126 A CN103288126 A CN 103288126A CN 2013101772832 A CN2013101772832 A CN 2013101772832A CN 201310177283 A CN201310177283 A CN 201310177283A CN 103288126 A CN103288126 A CN 103288126A
- Authority
- CN
- China
- Prior art keywords
- titanium dioxide
- dioxide nanotube
- titania nanotube
- powder
- cats product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention discloses a method of preparing a titanium dioxide nanotube with assistance of a cationic surface active agent. The method comprises: adding titanium dioxide powder and hexadecyl trimethyl ammonium bromide into a polytetrafluoroethylene hydrothermal reaction kettle filled with a strong base solution according to a weight ratio of 1:1-1:5, uniformly mixing the ingredients, reacting at 100-200 DEG C for 15-30hours, performing acid treatment, washing, filtering, drying and burning the ingredients to obtain the titanium dioxide nanotube. The titanium dioxide nanotube is efficiently prepared by a soft template combining with a hydrothermal method. The length of the prepared titanium dioxide nanotube is hundreds of nanometers, the outside diameter is about 10nm, the inside diameter is about 5nm, the titanium dioxide nanotube contains 2-5 layers of tube walls and two open ends. Compared with the titanium dioxide nanotube prepared by a common hydrothermal method under the same condition, the tube length is obviously increased, the tube diameter is more uniform, the draw ratio is large, the tube forming efficiency is high and the aggregation condition is alleviated, thereby being very beneficial for application of the titanium dioxide nanotube in various fields.
Description
Technical field
What the present invention relates to is a kind of preparation of nanomaterials, specifically a kind of preparation method of titania nanotube.
Background technology
Titanic oxide nano is a kind of important inorganic functional material, have nontoxic, excellent specific property such as chemical stability is high, air-sensitive, opto-electronic conversion effect, catalytic activity are good, be widely used in fields such as coating, semiconductor components and devices, catalysis, solar cell, gas sensor at present.
Titania nanotube is the another kind of existence form of titanium dioxide, because its specific surface area is big, have higher adsorptive power and have significant dimensional effect, can further improve the photoelectric properties of titanium dioxide and catalytic activity etc., have higher using value.
The preparation method of titania nanotube mainly contains three kinds: (1) anonizing, this method are that metal titanium sheet is immersed the nanotube that obtains to align at the titanium sheet growth in the electrolytic solution through corrosion.(2) hard template method be template with the nano-form of porous alumina (PAA), photoetch preparation, polycarbonate nano filter membrane etc., prepares titania nanotube by sol-gel method, solution impregnation-hot melt solution, electrodip process etc.(3) hydrothermal method joins a certain amount of titania powder in the dense strong base solution and to get titania nanotube in 100～200 ℃ of hydro-thermal reaction for some time.This method is compared with preceding two kinds of methods, topmost characteristics are to be Powdered on the nanotube macroscopic view for preparing, and have widened its Application Areas, and operating procedure is simple in addition, advantages such as the nanotube caliber of preparation is less have become the topmost method for preparing titania nanotube at present.Tube efficiency is low, the nanotube of preparation is short and easy subject matter such as reunion but this method exists into.Document Wang, M.; Guo, D.-j.; Li, H.-l., High activity of novel Pd/TiO
2Nanotube catalysts for methanol electro-oxidation.Journal of Solid State Chemistry2005,178 (6), 1996-2000; Abida, B.; Chirchi, L.; Baranton, S.; Napporn, T.W.; Kochkar, H.; L é ger, J.-M.; Ghorbel, A., Preparation and characterization of Pt/TiO
2Nanotubes catalyst for methanol electro-oxidation.Applied Catalysis B:Environmental2011,106 (3-4), 609-615 and document Xu, Y.-H.; Chen, C.; Yang, X.-L.; Li, X.; Wang, B.-F., Preparation, characterization and photocatalytic activity of the neodymium-doped TiO
2Nanotubes.Applied Surface Science2009,255 (20), 8624-8628 does not use tensio-active agent, adopts the titania nanotube of common Hydrothermal Preparation, and length only is tens nanometers.Document Xiao, N.; Li, Z.; Liu, J.; Gao, Y., Effects of calcination temperature on the morphology, structure and photocatalytic activity of titanate nanotube thin films.Thin Solid Films2010,519 (1), 541-548 uses metal titanium sheet to make presoma, adopts the titania nanotube of common Hydrothermal Preparation to be intertwined, and is dispersed relatively poor.Document Wang, H.; Chen, X.; Weng, X.; Liu, Y.; Gao, S.; Wu, Z., Enhanced catalytic activity for selective catalytic reduction of NO over titanium nanotube-confined CeO
2Catalyst.Catalysis Communications2011,12 (11), the nanotube of 1042-1045. preparation is same reunites together, and becomes tube efficiency lower.
At present, tensio-active agent has been used as soft template and has prepared nano materials such as nanometer rod, nanotube, but tensio-active agent helps the efficient production titania nanotube that report is not also arranged.How to be prepared into tube efficiency height and size pattern preferably the titania nanotube powder become problem demanding prompt solution.
Summary of the invention
The object of the present invention is to provide a kind of one-tenth tube efficiency height, the size pattern of product is the method for cats product aid preparation titania nanotube preferably.
The object of the present invention is achieved like this:
Be that the ratio of 1:1-1:5 joins in the tetrafluoroethylene hydrothermal reaction kettle that fills strong base solution with titania powder and cetyl trimethylammonium bromide according to weight ratio, mix the back and carry out acid treatment in reaction under the 100-200 ℃ of temperature after 15-30 hour, washing, filter, oven dry obtains titania nanotube after the calcining.
The present invention can also comprise:
1, the particle diameter of described titania powder is 10～100nm, and crystal formation is anatase octahedrite phase, rutile phase or the two mixture.
2, described alkaline solution is that concentration is the NaOH solution of 8-15mol/L.
3, the raw material constitutive molar ratio is TiO
2: CTAB:NaOH:H
2O=1:0.01～1:5～100:50～1500.
4, titania powder and cetyl trimethylammonium bromide adopt ultrasonic method to carry out dispersing and mixing in concentrated alkali solution.
5, ultrasonic power is 100～500W, and the time is 0.5h～3h.
6, described acid-treated detailed process is that the nitric acid of 0.1～1.0mol/L or hydrochloric acid are joined in the powder of reaction gained 50～100 ℃ of ultrasonic 1～3h.
7, calcining temperature is 400～800 ℃, and the time is 1～5h.
The present invention adopts soft template and the hydrothermal method titania nanotube that combined efficient production.The long hundreds of nanometer of gained titania nanotube, the about 10nm of external diameter, the about 5nm of internal diameter have 2-5 layer tube wall, both ends open.Compare with the titania nanotube that common hydro-thermal legal system under the same terms gets, pipe range obviously increases, and caliber is more even, and length-to-diameter ratio is big, becomes the tube efficiency height, and the reunion situation alleviates, and is all very favourable to its application in every respect.
Description of drawings
Fig. 1 is the titania nanotube TEM figure of common Hydrothermal Preparation.
Fig. 2 is the titania nanotube TEM figure of the used soft template-Hydrothermal Preparation of the present invention under the same terms.
Fig. 3, Fig. 4 are the titania nanotube HRTEM figure of the used soft template-Hydrothermal Preparation of the present invention.
Embodiment
Below in conjunction with example technical scheme of the present invention and effect are further described.But employed concrete grammar, prescription and explanation are not limitation of the present invention.
Embodiment one:
Step 1, configuration 10-50mL concentration are that the NaOH solution of 8-15mol/L joins in the tetrafluoroethylene inner liner of reaction kettle.
Step 2, weighing 0.1-10g cetyl trimethylammonium bromide, 0.1-3g particle diameter are that 10-100nm, crystal formation are the titanic oxide nano powder of anatase octahedrite phase, rutile phase or the two mixture, and sonic oscillation makes it to mix in the concentrated alkali solution that adding prepares.
Step 3 is put into baking oven in 100-200 ℃ of hydro-thermal reaction 15-30h with stainless steel cauldron.
Step 4 after hydro-thermal reaction finishes, is poured out supernatant liquor, and washing gained pressed powder is to neutral.
Step 5, in the powder that nitric acid or the hydrochloric acid of 0.1-1mol/L is joined gained, 50-100 ℃ of ultrasonic 1-3h.
Step 6 is washed the sample after the acid treatment approaching neutral.
Step 7 is filtered.
Step 8, the gained powder is fully dry.
Step 9 is calcined 1-5h with dried powder in 400-800 ℃.
Embodiment two:
Configuration 20mL concentration is that the NaOH solution of 10mol/L joins in the tetrafluoroethylene inner liner of reaction kettle.
Weighing 0.5g cetyl trimethylammonium bromide, 1g particle diameter are the anatase phase titanium dioxide powder of 20nm, and sonic oscillation makes it to mix in the concentrated alkali solution that adding prepares, in 120 ℃ of hydro-thermal reaction 30h.
After hydro-thermal reaction finishes, supernatant liquor is poured out, washing gained pressed powder is to neutral.
The nitric acid of 0.1mol/L is joined in the powder of gained 60 ℃ of ultrasonic 2h.
Powder after the acid treatment is washed approaching neutrality, filter, fully dry.
Dried powder is ground the back in 400 ℃ of calcining 2h.
Can the described titania nanotube of efficient production with aforesaid method.
Claims (6)
1. the method for a cats product aid preparation titania nanotube, it is characterized in that: be that the ratio of 1:1-1:5 joins in the tetrafluoroethylene hydrothermal reaction kettle that fills strong base solution with titania powder and cetyl trimethylammonium bromide according to weight ratio, mix the back and carry out acid treatment in reaction under the 100-200 ℃ of temperature after 15-30 hour, washing, filter, oven dry obtains titania nanotube after the calcining.
2. the method for cats product aid preparation titania nanotube according to claim 1, it is characterized in that: the particle diameter of described titania powder is 10～100nm, crystal formation be anatase octahedrite phase, rutile mutually or the two mixture.
3. the method for cats product aid preparation titania nanotube according to claim 2, it is characterized in that: described alkaline solution is that concentration is the NaOH solution of 8-15mol/L.
4. the method for cats product aid preparation titania nanotube according to claim 3, it is characterized in that: titania powder and cetyl trimethylammonium bromide adopt ultrasonic method to carry out dispersing and mixing in concentrated alkali solution; Ultrasonic power is 100～500W, and the time is 0.5h～3h.
5. the method for cats product aid preparation titania nanotube according to claim 4, it is characterized in that: described acid-treated detailed process is that the nitric acid of 0.1～1.0mol/L or hydrochloric acid are joined in the powder of reaction gained 50～100 ℃ of ultrasonic 1～3h.
6. the method for cats product aid preparation titania nanotube according to claim 5, it is characterized in that: calcining temperature is 400～800 ℃, the time is 1～5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101772832A CN103288126A (en) | 2013-05-14 | 2013-05-14 | Method of preparing titanium dioxide nanotube with assistance of cationic surface active agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101772832A CN103288126A (en) | 2013-05-14 | 2013-05-14 | Method of preparing titanium dioxide nanotube with assistance of cationic surface active agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103288126A true CN103288126A (en) | 2013-09-11 |
Family
ID=49089741
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101772832A Pending CN103288126A (en) | 2013-05-14 | 2013-05-14 | Method of preparing titanium dioxide nanotube with assistance of cationic surface active agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103288126A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553127A (en) * | 2013-10-22 | 2014-02-05 | 渤海大学 | Method for preparing anatase type titanium dioxide nano tube |
| CN104386743A (en) * | 2014-11-26 | 2015-03-04 | 上海大学 | Solvothermal preparation method of anatase type TiO2 nanometer tube |
| CN104986777A (en) * | 2015-05-25 | 2015-10-21 | 哈尔滨工程大学 | Method for preparation of double-wall Na2(TiO)SiO4 nanotube |
| CN105080498A (en) * | 2014-05-21 | 2015-11-25 | 江苏瑞丰科技实业有限公司 | Multifunctional high-efficiency integrated air pollution processing material |
| CN105158236A (en) * | 2015-08-03 | 2015-12-16 | 济南大学 | Preparation method of electrochemiluminescence sensor for detecting benzoapyrene |
| CN105962282A (en) * | 2016-05-03 | 2016-09-28 | 王胜 | Plant salt containing sea salt and aloe gelatin and method for preparing plant salt containing sea salt and aloe gelatin |
| CN106012051A (en) * | 2016-07-29 | 2016-10-12 | 爱芯环保科技（厦门）股份有限公司 | Photocatalyst fiber preparation device and method |
| CN106118329A (en) * | 2016-07-06 | 2016-11-16 | 铜陵青铜时代雕塑有限公司 | A kind of indoor copper sculpture epoxy acrylic anticorrosion water-soluble paint containing Oleum Santali albi and preparation method thereof |
| CN106118330A (en) * | 2016-07-06 | 2016-11-16 | 铜陵青铜时代雕塑有限公司 | A kind of high pliable and tough cracking resistance copper sculpture epoxy acrylic anticorrosion water-soluble paint and preparation method thereof |
| CN107217287A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| 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 |
| CN108855031A (en) * | 2018-07-24 | 2018-11-23 | 陕西麦可罗生物科技有限公司 | A kind of nano-tube material and preparation method of suitable kasugarnycin wastewater treatment |
| CN111841517A (en) * | 2020-07-16 | 2020-10-30 | 安徽元琛环保科技股份有限公司 | Preparation method of titanium dioxide carrier for denitration catalyst and carrier prepared by preparation method |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1528672A (en) * | 2003-09-26 | 2004-09-15 | 清华大学 | Titanium oxide nano tube and preparing method thereof |
| CN101234781A (en) * | 2008-02-29 | 2008-08-06 | 福州大学 | Method for preparing high pure brookite type titanium dioxide nano-tube |
| 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 |
-
2013
- 2013-05-14 CN CN2013101772832A patent/CN103288126A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1528672A (en) * | 2003-09-26 | 2004-09-15 | 清华大学 | Titanium oxide nano tube and preparing method thereof |
| CN101234781A (en) * | 2008-02-29 | 2008-08-06 | 福州大学 | Method for preparing high pure brookite type titanium dioxide nano-tube |
| 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 |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553127A (en) * | 2013-10-22 | 2014-02-05 | 渤海大学 | Method for preparing anatase type titanium dioxide nano tube |
| CN103553127B (en) * | 2013-10-22 | 2015-11-25 | 渤海大学 | The preparation method of anatase type titanium dioxide nano tube |
| CN105080498A (en) * | 2014-05-21 | 2015-11-25 | 江苏瑞丰科技实业有限公司 | Multifunctional high-efficiency integrated air pollution processing material |
| CN105080498B (en) * | 2014-05-21 | 2018-04-10 | 江苏瑞丰科技实业有限公司 | Multifunctional efficient Integral air pollution processing material |
| CN104386743A (en) * | 2014-11-26 | 2015-03-04 | 上海大学 | Solvothermal preparation method of anatase type TiO2 nanometer tube |
| CN104386743B (en) * | 2014-11-26 | 2016-04-27 | 上海大学 | A kind of Detitanium-ore-type TiO 2the solvothermal preparation method of nanotube |
| CN104986777A (en) * | 2015-05-25 | 2015-10-21 | 哈尔滨工程大学 | Method for preparation of double-wall Na2(TiO)SiO4 nanotube |
| CN104986777B (en) * | 2015-05-25 | 2017-05-24 | 哈尔滨工程大学 | Method for preparation of double-wall Na2(TiO)SiO4 nanotube |
| CN105158236A (en) * | 2015-08-03 | 2015-12-16 | 济南大学 | Preparation method of electrochemiluminescence sensor for detecting benzoapyrene |
| CN105962282A (en) * | 2016-05-03 | 2016-09-28 | 王胜 | Plant salt containing sea salt and aloe gelatin and method for preparing plant salt containing sea salt and aloe gelatin |
| CN106118330A (en) * | 2016-07-06 | 2016-11-16 | 铜陵青铜时代雕塑有限公司 | A kind of high pliable and tough cracking resistance copper sculpture epoxy acrylic anticorrosion water-soluble paint and preparation method thereof |
| CN106118329A (en) * | 2016-07-06 | 2016-11-16 | 铜陵青铜时代雕塑有限公司 | A kind of indoor copper sculpture epoxy acrylic anticorrosion water-soluble paint containing Oleum Santali albi and preparation method thereof |
| CN106012051A (en) * | 2016-07-29 | 2016-10-12 | 爱芯环保科技（厦门）股份有限公司 | Photocatalyst fiber preparation device and method |
| CN107217287A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| 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 |
| CN108855031A (en) * | 2018-07-24 | 2018-11-23 | 陕西麦可罗生物科技有限公司 | A kind of nano-tube material and preparation method of suitable kasugarnycin wastewater treatment |
| CN108855031B (en) * | 2018-07-24 | 2021-06-11 | 陕西麦可罗生物科技有限公司 | Nanotube material suitable for kasugamycin wastewater treatment and preparation method thereof |
| CN111841517A (en) * | 2020-07-16 | 2020-10-30 | 安徽元琛环保科技股份有限公司 | Preparation method of titanium dioxide carrier for denitration catalyst and carrier prepared by preparation method |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103288126A (en) | Method of preparing titanium dioxide nanotube with assistance of cationic surface active agent | |
| Nguyen et al. | Perovskite oxide-based photocatalysts for solar-driven hydrogen production: Progress and perspectives | |
| Yu et al. | Single-crystalline TiO2 nanorods: Highly active and easily recycled photocatalysts | |
| Yan et al. | Facile synthesis of an iron doped rutile TiO 2 photocatalyst for enhanced visible-light-driven water oxidation | |
| CN104671282B (en) | A kind of preparation method of composite titania material hollow ball | |
| CN104192899B (en) | One prepares TiO2The method of nano crystal particles | |
| CN101525152B (en) | Mumm-shaped 3D TiO nanometer material and preparation method thereof | |
| CN100546915C (en) | A kind of preparation method of anatase-like titanium dioxide nanometer powder | |
| CN101508464A (en) | Process for preparing anatase type nano-titanium dioxide | |
| Kiatkittipong et al. | Photocatalysis of heat treated sodium-and hydrogen-titanate nanoribbons for water splitting, H2/O2 generation and oxalic acid oxidation | |
| CN104096552A (en) | Denitration titanium dioxide with specific surface higher than 350 m<2>/g and preparation method thereof | |
| CN104760995B (en) | A kind of preparation method of brookite titania nanorod | |
| CN105344350A (en) | Preparation method for molybdenum-doped TiO2 nanowire/graphene compound with high catalytic degradation activity under visible light | |
| CN104226320B (en) | The preparation method of vanadium boron codope titanium dioxide and nickel oxide composite photo-catalyst | |
| Garay-Rodríguez et al. | Photocatalytic evaluation of composites of Ba3Li2Ti8O20-CuO in the reduction of CO2 to formaldehyde under visible light irradiation | |
| CN101698504A (en) | Method for synthesizing nano titanium dioxide through microwaves | |
| CN104310466A (en) | Hollow titanium dioxide microsphere based on gel sphere precursor and preparation method of hollow titanium dioxide microsphere | |
| CN103601239A (en) | Preparation method of anatase and brookite mixed crystal TiO2 nanowire | |
| CN102161506B (en) | Method for preparing C-N-codoped nano-TiO2 powder | |
| CN102502871B (en) | Method for synthesizing three-dimensional porous ferric oxide nano rod cluster | |
| He et al. | In situ synthesis of the mesoporous C–TiO2 microspheres derived from partial hydrolysis tetrabutyl titanate for enhanced photocatalytic degradation under visible light | |
| Moghaddam et al. | Ultrasonic wave effects on the diameter of TiO2 nanoparticles | |
| CN102730753A (en) | Method for preparing anatase porous TiO2 spheres, core-shell structure and hollow spheres | |
| CN103395831A (en) | Hydrothermal preparation method of shape-controllable titanium dioxide nano tube | |
| CN104986777B (en) | Method for preparation of double-wall Na2(TiO)SiO4 nanotube |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130911 |