CN103601239A - A kind of preparation method of mixed crystal TiO2 nanowire of anatase and brookite - Google Patents
A kind of preparation method of mixed crystal TiO2 nanowire of anatase and brookite Download PDFInfo
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- CN103601239A CN103601239A CN201310592566.3A CN201310592566A CN103601239A CN 103601239 A CN103601239 A CN 103601239A CN 201310592566 A CN201310592566 A CN 201310592566A CN 103601239 A CN103601239 A CN 103601239A
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- anatase
- brookite
- mixed
- tio
- mixed crystal
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 239000013078 crystal Substances 0.000 title claims abstract description 30
- 239000002070 nanowire Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 230000007935 neutral effect Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 4
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims abstract 4
- 239000011259 mixed solution Substances 0.000 claims abstract 2
- 238000002525 ultrasonication Methods 0.000 claims abstract 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000005755 formation reaction Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种锐钛矿和板钛矿的混晶TiO2纳米线的制备方法，属于TiO2纳米材料技术领域。该方法过程包括：在NaOH溶液中加入锐钛矿和金红石混晶的P25颗粒，经过超声，搅拌混合均匀，将混合溶液在温度为180-200℃进行水热反应24～48h，然后自然冷却至室温，反应产物用去离子水洗涤至中性，用HCl搅拌洗涤，再用去离子水洗涤至中性，然后在空气中干燥，最后将产物以一定速率升温至500℃～550℃煅烧，得到锐钛矿与板钛矿混合晶型的TiO2纳米线。本发明优点：制备工艺简单，制备的TiO2纳米线含有板钛矿和锐钛矿两种晶型，该混晶的TiO2纳米线具有良好的光催化性能。The invention discloses a method for preparing anatase and brookite mixed-crystal TiO2 nanowires, belonging to the technical field of TiO2 nanometer materials. The method process includes: adding P25 particles of anatase and rutile mixed crystals to NaOH solution, stirring and mixing evenly through ultrasonication, carrying out hydrothermal reaction of the mixed solution at a temperature of 180-200°C for 24-48 hours, and then naturally cooling to At room temperature, the reaction product is washed with deionized water until neutral, stirred and washed with HCl, then washed with deionized water until neutral, then dried in the air, and finally the product is heated to 500°C to 550°C at a certain rate for calcination to obtain Anatase and Brookite Mixed TiO 2 Nanowires. The invention has the advantages that the preparation process is simple, the prepared TiO2 nanowire contains brookite and anatase crystal forms, and the mixed crystal TiO2 nanowire has good photocatalytic performance.
Description
Technical field
The present invention relates to the mixed crystal TiO of a kind of anatase octahedrite and brookite
2the preparation method of nano wire, belongs to TiO
2technical field of nano material.
Background technology
In the modern life, energy shortage and environmental pollution become the problem that people pay special attention to.Photocatalitic Technique of Semiconductor can directly utilize sun power to realize water decomposition to prepare clean energy hydrogen, decomposing organic pollutant or CO2 is reduced into hydrocarbon fuels, thereby is considered to effectively to solve the green method of energy environment issues.In numerous photocatalyst materials, TiO
2due to its at a low price, nontoxic, stable chemical nature, catalytic activity is good, oxidation capacity advantages of higher obtains people common concern, for TiO
2research be also the focus in this field always.
The photocatalytic activity of semiconductor material is determined by many factors such as the crystal formation, lattice defect, degree of crystallinity, material specific surface area of material conventionally jointly, and wherein crystal formation is an extremely important factor.TiO
2have three kinds of crystal formations: anatase octahedrite, rutile and brookite.Detitanium-ore-type TiO
2energy gap be 3.2 eV, there is good photocatalytic activity; Rutile TiO
2energy gap be 3.0 eV, ultraviolet ray is had to good shielding effect and chemical stability; Brookite type TiO
2structure is stable not, so Detitanium-ore-type TiO
2and rutile TiO
2the most frequently used TiO
2, for example Degussa P25 is the mixed crystal type TiO that the ratio of Anatase and Rutile Type is approximately 4:1
2, be also most widely used mixed crystal TiO
2product.Aspect photochemical catalysis, mixed crystal TiO
2exist " Mixed crystal effect ", the active TiO that often surpasses monocrystalline phase
2.
Prepare at present mixed crystal TiO
2one of method be vapor phase process, P25 for example; Other method is mainly with TiCl
4or tetrabutyl titanate is raw material, adopt the method for sol-gel or hydro-thermal, the TiO preparing
2mostly be the mixed phase of rutile and two kinds of crystal formations of anatase octahedrite, and pattern is mostly nano particle.
Summary of the invention
The object of the present invention is to provide a kind of anatase octahedrite and brookite mixed crystal TiO
2the preparation method of nano wire, this preparation method's process is simple, the TiO of prepared anatase octahedrite and brookite mixed crystal
2nano wire has higher photocatalysis performance.
The present invention is achieved by the following technical solutions, a kind of anatase octahedrite and brookite mixed crystal TiO
2the preparation method of nano wire, is characterized in that comprising following process:
NaOH is dissolved in to deionized water, and compound concentration is the NaOH solution of 8～12 mol/L, pressing NaOH in solution is 16:1 with the P25 granular mass ratio of anatase octahedrite and rutile-type mixed crystal, the P25 particle of anatase octahedrite and rutile-type mixed crystal is joined in NaOH solution, through ultrasonic, be uniformly mixed, mixing solutions is carried out under 180～200 ℃ of conditions to hydro-thermal reaction 24～48 h, then naturally cool to room temperature, reaction product is extremely neutral with deionized water wash, by concentration, be after the HCl agitator treating of 0.1 mol/L again, extremely neutral with deionized water wash, after air drying, product is risen to 500～550 ℃ of calcining 3 h with the speed of 5 ℃/min, obtain the TiO of anatase octahedrite and brookite mixing crystal formation
2nano wire.
The present invention has the following advantages: preparation technology is simple, the TiO of preparation
2nano wire contains brookite and two kinds of crystal formations of anatase octahedrite, the TiO of this mixed crystal
2nano wire has good photocatalysis performance.
Accompanying drawing explanation
Fig. 1 is the prepared TiO of embodiment mono-
2the SEM figure of nano wire.
Fig. 2 is the prepared TiO of embodiment mono-
2the TEM figure of nano wire.
Fig. 3 is the prepared TiO of embodiment mono-
2the XRD figure of nano wire.
In figure: ■ represents anatase octahedrite composition; ▲ represent brookite composition.
Embodiment
Below in conjunction with example, the present invention will be further described, and these examples, just for the present invention is described, do not limit the present invention.
Embodiment mono-
Prepare the NaOH solution that 80 mL concentration are 10 mol/L; Take the P25 powder of 2 g anatase octahedrites and rutile mixed crystal, join in NaOH solution, ultrasonic 30 min, stir 30 min, and solution mixes; Subsequently the solution preparing is transferred in hydrothermal reaction kettle, put into baking oven at 200 ℃ of reaction 24 h; After hydro-thermal reaction finishes, product in reactor is washed till to neutrality with deionized water, by product stirring and pickling 5 h in the hydrochloric acid soln of 0.1 mol/L, with deionized water, product is washed till to neutrality more subsequently, in air, dry, finally product is warming up to 500 ℃ of calcining 3 h with 5 ℃/min, obtains the TiO of anatase octahedrite and brookite mixed crystal
2nano wire.
Embodiment bis-
The present embodiment is identical with embodiment mono-step, and difference is: the P25 powder quality taking is become to 2.4 g from 2 g, and the hydro-thermal reaction time becomes 48 h from 24 h.
Embodiment tri-
The present embodiment is identical with embodiment mono-step, and difference is: hydrothermal temperature is become to 180 ℃ from 200 ℃, and the hydro-thermal reaction time becomes 48 h from 24 h, and calcining temperature becomes 550 ℃ from 500 ℃.
Embodiment tetra-
The present embodiment is identical with embodiment mono-step, and difference is: the stirring and pickling time in the hydrochloric acid at 0.1 mol/L is become to 3 h from 5 h, and calcination time becomes 2 h from 3 h.
Claims (1)
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| CN201310592566.3A CN103601239A (en) | 2013-11-22 | 2013-11-22 | A kind of preparation method of mixed crystal TiO2 nanowire of anatase and brookite |
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|---|---|---|---|
| CN201310592566.3A CN103601239A (en) | 2013-11-22 | 2013-11-22 | A kind of preparation method of mixed crystal TiO2 nanowire of anatase and brookite |
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|---|---|
| CN103601239A true CN103601239A (en) | 2014-02-26 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525168A (en) * | 2014-12-18 | 2015-04-22 | 黑龙江大学 | Method for synthesizing anatase/brookite nano composite material for photocatalytic decomposition of water into hydrogen through one-step hydrothermal method |
| CN105776327A (en) * | 2016-03-25 | 2016-07-20 | 武汉理工大学 | Brookite and anatase mixed-phase TiO2 micron hollow spheres assembled by nanorods and its preparation method and application |
| CN106975488A (en) * | 2016-01-15 | 2017-07-25 | 上海乐泽环境工程有限公司 | It is a kind of that aluminium-nano-TiO is activated with Ni-2For the efficient elctro-catalyst of active centre |
| CN108097225A (en) * | 2017-11-23 | 2018-06-01 | 昆明理工大学 | A kind of method that crystal type nano TiO 2 is prepared using seed crystal induction |
| CN111617760A (en) * | 2020-06-29 | 2020-09-04 | 盐城工学院 | A kind of Mn-TiO2 composite photocatalytic material and its preparation method and application |
Citations (3)
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|---|---|---|---|---|
| CN1613585A (en) * | 2004-11-09 | 2005-05-11 | 北京航空航天大学 | Method for preparing titania wiring pipe and use for wiring pipe |
| CN101920990A (en) * | 2010-07-23 | 2010-12-22 | 上海师范大学 | A method for preparing titanium dioxide nanowires by high-pressure microwave method |
| CN102774882A (en) * | 2012-07-05 | 2012-11-14 | 常州大学 | Method for preparing candied haw-shaped pure anatase type nano-titania wire in larger scale |
-
2013
- 2013-11-22 CN CN201310592566.3A patent/CN103601239A/en active Pending
Patent Citations (3)
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| CN1613585A (en) * | 2004-11-09 | 2005-05-11 | 北京航空航天大学 | Method for preparing titania wiring pipe and use for wiring pipe |
| CN101920990A (en) * | 2010-07-23 | 2010-12-22 | 上海师范大学 | A method for preparing titanium dioxide nanowires by high-pressure microwave method |
| CN102774882A (en) * | 2012-07-05 | 2012-11-14 | 常州大学 | Method for preparing candied haw-shaped pure anatase type nano-titania wire in larger scale |
Non-Patent Citations (3)
| Title |
|---|
| C. GUO ET AL.: "Photodegradation of rhodamine B and methyl orange over one-dimensional TiO2 catalysts under simulated solar irradiation", 《APPLIED SURFACE SCIENCE》 * |
| H. YU ET AL.: "Photocatalytic activity of the calcined H-titanate nanowires for photocatalytic oxidation of acetone in air", 《CHEMOSPHERE》 * |
| N. VIRIYA-EMPIKUL ET AL.: "Effect of preparation variables on morphology and anatase-brookite phase transition in sonication assisted hydrothermal reaction for synthesis of titanate nanostructures", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525168A (en) * | 2014-12-18 | 2015-04-22 | 黑龙江大学 | Method for synthesizing anatase/brookite nano composite material for photocatalytic decomposition of water into hydrogen through one-step hydrothermal method |
| CN106975488A (en) * | 2016-01-15 | 2017-07-25 | 上海乐泽环境工程有限公司 | It is a kind of that aluminium-nano-TiO is activated with Ni-2For the efficient elctro-catalyst of active centre |
| CN105776327A (en) * | 2016-03-25 | 2016-07-20 | 武汉理工大学 | Brookite and anatase mixed-phase TiO2 micron hollow spheres assembled by nanorods and its preparation method and application |
| CN105776327B (en) * | 2016-03-25 | 2017-09-29 | 武汉理工大学 | A kind of brockite and anatase mixed phase TiO of nanometer rods assembling2Micrometre hollow sphere and its preparation method and application |
| CN108097225A (en) * | 2017-11-23 | 2018-06-01 | 昆明理工大学 | A kind of method that crystal type nano TiO 2 is prepared using seed crystal induction |
| CN108097225B (en) * | 2017-11-23 | 2021-05-14 | 昆明理工大学 | A kind of method utilizing seed crystal induction to prepare crystalline nanometer titanium dioxide |
| CN111617760A (en) * | 2020-06-29 | 2020-09-04 | 盐城工学院 | A kind of Mn-TiO2 composite photocatalytic material and its preparation method and application |
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Application publication date: 20140226 |