CN101444723A - Method for preparing TiO2 hollow micro-sphere material - Google Patents
Method for preparing TiO2 hollow micro-sphere material Download PDFInfo
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- CN101444723A CN101444723A CNA2008100413390A CN200810041339A CN101444723A CN 101444723 A CN101444723 A CN 101444723A CN A2008100413390 A CNA2008100413390 A CN A2008100413390A CN 200810041339 A CN200810041339 A CN 200810041339A CN 101444723 A CN101444723 A CN 101444723A
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Abstract
The invention discloses a method for preparing TiO2 hollow micro-sphere material which belongs to the technical field of preparing semiconductor photocatalysis material. In the method, titanium potassium oxalate, oxyful and concentrated hydrochloric acid are used as materials, and a hydrothermal synthesis method and the oxygen released in the reaction process are used as a template to prepare the TiO2 hollow micro-sphere material. The method has the advantages of simple operation, low reaction temperature and short reaction time; besides, the method takes the oxygen generated during the reaction process as the template, and does not need to include the techniques of specially preparing the template or removing the template in the preparing process; the whole preparing process is quite simple. The specific area of the prepared material is high; and the material is applied on the aspects of sterilization and gas storage in environment protection especially.
Description
Technical field
The present invention relates to a kind of TiO
2The hollow microsphere preparation methods, being specifically related to a kind of is the TiO of template with gas
2The hollow microsphere preparation methods, the technical field of genus conductor photocatalysis material.
Background technology
TiO
2Be a kind of important multifunctional inorganic material, it has broad application prospects in fields such as gas sensor, contaminant degradation, solar hydrogen making, solar cells.Recent two decades, people utilize the whole bag of tricks (hydrothermal synthesis method, vapor deposition method, template, galvanoplastic etc.) successfully to prepare TiO
2Nanosphere, nanometer rods, materials such as nanotube and nano-rings, and TiO
2The preparation of hollow microsphere material then is a bigger challenge.
At present, hollow ball nano particle (Hollow spheres) has been represented a material colony, it be meant a class size nanometer to the micron between the material with special construction.Because the hollow space of this class material can hold a large amount of guest molecules or large-sized object, thereby produces some peculiar effects.Over past ten years, the hollow ball material is one of focus of studying of people always.Because it is low that this class material has density, specific area is big, good stability and characteristics with surface seepage ability, therefore in fields such as chemistry, biology and material science important use is arranged all, as control release capsule (medicine, pigment, cosmetics, printing ink), artificial cell, electricity component, filler, catalysis, parting material, coating and Accoustical sound proofing material etc.
Existing TiO
2The hollow microsphere preparation methods mostly is template with the organic matter, and the technology of the preparation of template and removal is also quite complicated, is not suitable for industrialized production.
Summary of the invention
The purpose of this invention is to provide a kind of TiO
2The hollow microsphere preparation methods.This method has that operation is simple, makes the TiO of material
2The aperture of hollow microsphere is even, is about 2 μ m, makes material and has the advantage of monocrystalline preferably.
For realizing above purpose, the technical solution used in the present invention is to be raw material with titanium potassium oxalate, hydrogen peroxide and concentrated hydrochloric acid, is template with hydrothermal synthesis method with the oxygen that discharges in the course of reaction, preparation TiO
2The hollow microsphere material.
Now describe technical scheme of the present invention in detail.
A kind of TiO
2The hollow microsphere preparation methods is characterized in that, the concrete operations step:
The preparation of first step reaction solution
The titanium potassium oxalate of 0.708g is dissolved in the deionized water of 15ml, stirs, adding 15ml concentration is the hydrogen peroxide of 30wt%, adds the hydrochloric acid that 1～2ml concentration is 37wt% again, gets bolarious reaction solution;
The second step hydrothermal synthesis reaction
The bolarious reaction solution that the first step is made moves in the teflon-lined reactor, this reactor is put into baking oven, carry out hydrothermal synthesis reaction under 150 ℃, the oxygen that discharges in the course of reaction is as template, reacted eight hours, and naturally cooled to room temperature;
The processing of three-step reaction product
Clean second repeatedly with deionized water and go on foot the product that hydrothermal synthesis reaction generates, be neutral to it, centrifugation gets white product, in air and under 60 ℃, with this white product oven dry, gets the white powder TiO of 0.150g
2The hollow microsphere material.
Carry out the X-ray diffraction detection to making material, the characteristic peak numerical value of the PDF diffraction card anatase titanium dioxide 21-1272 sample that its characteristic peak numerical value and JCPDS publish fits like a glove, and illustrates that making material is anatase titanium dioxide.
Add hydrogen peroxide in the first step of the present invention, make reaction solution in the process of carrying out the second step hydrothermal synthesis reaction, can generate oxygen, as forming TiO
2Template during the hollow microsphere structure.The inner lining material of used reactor is a polytetrafluoroethylene (PTFE) in the 3rd step of the present invention, and during hydrothermal synthesis reaction, the maximum temperature that this reactor can bear is 180 ℃.
Compare with background technology, the present invention has following outstanding advantage:
1, operation is simple, do not use any large-scale instrument and equipment.
2, reaction temperature is lower, has only 150 ℃, and the reaction time is shorter, has only eight hours.
3, with the oxygen that generates in the course of reaction as template, need not comprise special preparation template in the preparation process and remove the technology of template that whole process of preparation is quite simple.
Description of drawings
Fig. 1 is TiO of the present invention
2The X-ray diffractogram of hollow microsphere material.
Fig. 2 a is TiO of the present invention
2One of SEM photo of hollow microsphere material.Among the figure, the TiO in the material
2The spheroid of hollow microsphere is more even.
Fig. 2 b is TiO of the present invention
2Two of the SEM photo of hollow microsphere material.A TiO is arranged at the middle part of figure
2Hollow microsphere opens osculum, and the inside that microballoon is described is empty.
Fig. 2 c is TiO of the present invention
2Three of the SEM photo of hollow microsphere material.This photo is taken after material is pulverized at material, can see clearly that from figure the spheroid inside of gained is empty, and the aperture is approximately 2 μ m.
The specific embodiment
Now further specify technical scheme of the present invention in conjunction with the accompanying drawings and embodiments.All embodiment all operate according to the described preparation method's of summary of the invention concrete operations step, and each embodiment is only enumerated the technical data of key separately.
Embodiment 1
In the first step, the addition of hydrochloric acid is 1ml.
Embodiment 2
In the first step, the addition of hydrochloric acid is 1.5ml.
Embodiment 3
In the first step, the addition of hydrochloric acid is 2ml.
Claims (1)
1, a kind of TiO
2The hollow microsphere preparation methods is characterized in that, the concrete operations step:
The preparation of first step reaction solution
The titanium potassium oxalate of 0.708g is dissolved in the deionized water of 15ml, stirs, adding 15ml concentration is the hydrogen peroxide of 30wt%, adds the hydrochloric acid that 1～2ml concentration is 37wt% again, gets bolarious reaction solution;
The second step hydrothermal synthesis reaction
The bolarious reaction solution that the first step is made moves in the teflon-lined reactor, this reactor is put into baking oven, carry out hydrothermal synthesis reaction under 150 ℃, the oxygen that discharges in the course of reaction is as template, reacted eight hours, and naturally cooled to room temperature;
The processing of three-step reaction product
Clean second repeatedly with deionized water and go on foot the product that hydrothermal synthesis reaction generates, be neutral to it, centrifugation gets white product, in air and under 60 ℃, with this white product oven dry, gets the white powder TiO of 0.150g
2The hollow microsphere material.
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| CNA2008100413390A CN101444723A (en) | 2008-08-04 | 2008-08-04 | Method for preparing TiO2 hollow micro-sphere material |
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| CNA2008100413390A CN101444723A (en) | 2008-08-04 | 2008-08-04 | Method for preparing TiO2 hollow micro-sphere material |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102765754A (en) * | 2012-07-20 | 2012-11-07 | 中国科学院金属研究所 | Method for preparing porous TiO2 quasi-monodispersed micron hollow spheres |
| CN102838162A (en) * | 2011-06-21 | 2012-12-26 | 中国科学院过程工程研究所 | Porous titanium dioxide hollow sphere, its preparation and method for adsorbing Cr(VI) |
| CN103058272A (en) * | 2011-10-19 | 2013-04-24 | 同济大学 | Method for preparing titanium dioxide hollow sphere with wide diameter distribution and high active surface orientation |
| CN105521774A (en) * | 2015-12-22 | 2016-04-27 | 镇江市高等专科学校 | Titanium dioxide hollow nano-material, and preparation method and application thereof |
| CN105540657A (en) * | 2016-01-14 | 2016-05-04 | 浙江大学 | Nanosheet-assembling core-shell structure anatase titanium dioxide microsphere and preparation method thereof |
| CN105600822A (en) * | 2016-03-31 | 2016-05-25 | 天津城建大学 | Preparation method of litchi-like hierarchical-structure {001}-surface-exposed TiO2 powder |
| CN106466604A (en) * | 2016-11-22 | 2017-03-01 | 安徽理工大学 | A kind of Cu2O/TiO2Composite photocatalyst material and preparation method thereof |
| CN107159192A (en) * | 2017-06-12 | 2017-09-15 | 青岛科技大学 | A kind of noble metal/TiO2Multilevel hierarchy of mixed crystal nanometer rods assembling and preparation method thereof |
| CN107224981A (en) * | 2017-06-26 | 2017-10-03 | 湖北大学 | A kind of titanium dioxide hollow ball load PdNi alloy nano catalyst and its preparation method and application |
| CN107233922A (en) * | 2017-06-19 | 2017-10-10 | 天津城建大学 | A kind of stone-like C2O7Ti2·3H2O photochemical catalysts and preparation method thereof |
| CN109331803A (en) * | 2018-10-11 | 2019-02-15 | 张润高 | Titanium dioxide-graphene composite material and its application in photo-catalytic nano colloidal sol |
| CN109365005A (en) * | 2018-10-11 | 2019-02-22 | 张润高 | High catalytic degradation performance Photocatalyst water colloidal sol and its production technology |
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2008
- 2008-08-04 CN CNA2008100413390A patent/CN101444723A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838162A (en) * | 2011-06-21 | 2012-12-26 | 中国科学院过程工程研究所 | Porous titanium dioxide hollow sphere, its preparation and method for adsorbing Cr(VI) |
| CN102838162B (en) * | 2011-06-21 | 2014-07-30 | 中国科学院过程工程研究所 | Porous titanium dioxide hollow sphere, its preparation and method for adsorbing Cr(VI) |
| CN103058272A (en) * | 2011-10-19 | 2013-04-24 | 同济大学 | Method for preparing titanium dioxide hollow sphere with wide diameter distribution and high active surface orientation |
| CN102765754A (en) * | 2012-07-20 | 2012-11-07 | 中国科学院金属研究所 | Method for preparing porous TiO2 quasi-monodispersed micron hollow spheres |
| CN105521774A (en) * | 2015-12-22 | 2016-04-27 | 镇江市高等专科学校 | Titanium dioxide hollow nano-material, and preparation method and application thereof |
| CN105540657A (en) * | 2016-01-14 | 2016-05-04 | 浙江大学 | Nanosheet-assembling core-shell structure anatase titanium dioxide microsphere and preparation method thereof |
| CN105600822A (en) * | 2016-03-31 | 2016-05-25 | 天津城建大学 | Preparation method of litchi-like hierarchical-structure {001}-surface-exposed TiO2 powder |
| CN106466604A (en) * | 2016-11-22 | 2017-03-01 | 安徽理工大学 | A kind of Cu2O/TiO2Composite photocatalyst material and preparation method thereof |
| CN107159192A (en) * | 2017-06-12 | 2017-09-15 | 青岛科技大学 | A kind of noble metal/TiO2Multilevel hierarchy of mixed crystal nanometer rods assembling and preparation method thereof |
| CN107159192B (en) * | 2017-06-12 | 2019-10-29 | 青岛科技大学 | A kind of noble metal/TiO2The preparation method of mixed crystal nanometer rods assembling multilevel structure |
| CN107233922A (en) * | 2017-06-19 | 2017-10-10 | 天津城建大学 | A kind of stone-like C2O7Ti2·3H2O photochemical catalysts and preparation method thereof |
| CN107233922B (en) * | 2017-06-19 | 2019-08-30 | 天津城建大学 | A kind of stone-like C2O7Ti2·3H2O photochemical catalyst and preparation method thereof |
| CN107224981A (en) * | 2017-06-26 | 2017-10-03 | 湖北大学 | A kind of titanium dioxide hollow ball load PdNi alloy nano catalyst and its preparation method and application |
| CN107224981B (en) * | 2017-06-26 | 2020-01-03 | 湖北大学 | PdNi alloy nano catalyst for ammonia borane hydrolysis hydrogen release and preparation method thereof |
| CN109331803A (en) * | 2018-10-11 | 2019-02-15 | 张润高 | Titanium dioxide-graphene composite material and its application in photo-catalytic nano colloidal sol |
| CN109365005A (en) * | 2018-10-11 | 2019-02-22 | 张润高 | High catalytic degradation performance Photocatalyst water colloidal sol and its production technology |
| CN109331803B (en) * | 2018-10-11 | 2021-09-03 | 林碧强 | Titanium dioxide-graphene composite material and application thereof in photocatalyst nano sol |
| CN109365005B (en) * | 2018-10-11 | 2021-09-17 | 浙江空将环境科技有限公司 | Photocatalyst hydrosol with high catalytic degradation performance and production process thereof |
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Open date: 20090603 |