CN105565375A - Preparing method for nanoscale porous titanium dioxide hollow spheres - Google Patents
Preparing method for nanoscale porous titanium dioxide hollow spheres Download PDFInfo
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- CN105565375A CN105565375A CN201410550111.XA CN201410550111A CN105565375A CN 105565375 A CN105565375 A CN 105565375A CN 201410550111 A CN201410550111 A CN 201410550111A CN 105565375 A CN105565375 A CN 105565375A
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- titanium dioxide
- porous titanium
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- hollow ball
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Abstract
The invention discloses a preparing method for nanoscale porous titanium dioxide hollow spheres. The preparing method is implemented according to the following steps that tetrabutyl titanate is hydrolyzed to obtain titanium dioxide sol; the obtained titanium dioxide sol is subjected to a hydrothermal reaction to obtain the nanoscale porous titanium dioxide hollow spheres. Tetrabutyl titanate is used as a precursor, and after tetrabutyl titanate is hydrolyzed, the nanoscale TiO2 porous hollow spheres are synthesized with ethyl alcohol as a solvothermal reaction medium and ammonium bicarbonate as a structural adjuvant. The synthesis method is simple in experiment process and free of environment pollution and is a relatively simple and environmental-friendly path, and it is unnecessary to remove a template.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, relate to a kind of preparation method of nanometer porous titanium dioxide hollow ball.
Background technology
In the last few years, nano material with its special structure and in optical, electrical, magnetic, chemistry etc. the performance of excellence attracted the sight of more and more investigator.Especially, nanometer titanic oxide material has been widely used in, in the middle of many fields, comprising chemical industry, environment protection, cosmetic industry and medical science etc.In order to improve the performance of titanic oxide material, comprise the different morphologies such as nano particle, nanotube, nanometer rod, nanometer ball own through succeeding in developing.Hollow structure material, as a kind of type material, has the advantage not available for a lot of solid material, such as: high-specific surface area, low density, excellent transmission perviousness, strong light capturing ability etc.Therefore, the preparation of hollow structure metal oxide materials has become the new problem of vast material scientific research personnel.
So far, although adopt different methods to prepare permitted eurypalynous titanium dioxide hollow sphere material, the problem such as there is technical process complexity, quality product has much room for improvement.
Summary of the invention
The object of this invention is to provide a kind of preparation method of nanometer porous titanium dioxide hollow ball, solve the problem that existing titanium dioxide hollow ball preparation technology flow process is complicated, quality product has much room for improvement.
The technical solution adopted in the present invention is, a kind of preparation method of nanometer porous titanium dioxide hollow ball, specifically implements according to the following steps:
Step 1,3 ~ 5:20:100 measures tetrabutyl titanate, dehydrated alcohol and deionized water by volume, adds in dehydrated alcohol by the tetrabutyl titanate measured, after mixing, instill under magnetic agitation in deionized water, hydrolysis generates oyster white TiO 2 sol, continues stirring 20 ~ 30min;
Step 2, by the TiO 2 sol washes of absolute alcohol generated in step 1, puts into tetrafluoroethylene water heating kettle liner, adds dehydrated alcohol and structure directing agent, stirs; Liner containing above-mentioned mixing solutions is placed in stainless steel outer sleeve obturage, puts into baking oven, take out after thermostatically heating certain hour and naturally cool to room temperature;
Step 3, opens kettle cover, removing supernatant liquid, through collected after centrifugation bottoms, then use deionized water and absolute ethanol washing hydrothermal product respectively by ultrasonic, centrifugal, finally product is placed in the dry 6h of baking oven, namely obtains nanometer porous titanium dioxide hollow ball.
Feature of the present invention is also,
Wherein in step 2, dehydrated alcohol addition is make mixed solution total amount reach 70 ~ 75% of tetrafluoroethylene water heating kettle total volume.
Wherein in step 2, structure directing agent is bicarbonate of ammonia, bicarbonate of ammonia and TiO 2 sol mass ratio 20 ~ 25:7.
Wherein in step 2, Heating temperature is 180 DEG C, and heat-up time is 45h ~ 48h.
Wherein in step 3, time of drying is 60 DEG C.
The invention has the beneficial effects as follows, the present invention utilizes tetrabutyl titanate as presoma, through hydrolysis after, ethanol be solvent thermal reaction medium, hydrogen-carbonate by under the condition for structure auxiliary, synthesized nano-TiO
2porous hollow sphere.This synthetic method experimentation is simple, without the need to removing template, and non-environmental-pollution, be a kind of approach of relatively simple and direct environmental protection.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
A preparation method for nanometer porous titanium dioxide hollow ball, specifically implements according to the following steps:
Step 1,3 ~ 5:20:100 measures tetrabutyl titanate, dehydrated alcohol and deionized water by volume, adds in dehydrated alcohol by the tetrabutyl titanate measured, after mixing, instill under magnetic agitation in deionized water, hydrolysis generates oyster white TiO 2 sol, continues stirring 20 ~ 30min;
Step 2, by the TiO 2 sol washes of absolute alcohol generated in step 1, puts into tetrafluoroethylene water heating kettle liner, 70% ~ 75% of total volume is added to dehydrated alcohol, by TiO 2 sol and bicarbonate of ammonia mass ratio 7:20 ~ 25, add bicarbonate of ammonia, stir.Liner containing above-mentioned mixing solutions is placed in stainless steel outer sleeve obturage, puts into baking oven, take out after constant temperature 180 DEG C heating 45h ~ 48h and naturally cool to room temperature;
Step 3, opens kettle cover, removing supernatant liquid, through collected after centrifugation bottoms, then use deionized water and absolute ethanol washing hydrothermal product respectively by ultrasonic, centrifugal, finally product is placed in 60 DEG C of dry 6h of baking oven, namely obtains nanometer porous titanium dioxide hollow ball.
Utilize tetrabutyl titanate as presoma, after hydrolysis, ethanol be solvent thermal reaction medium, hydrogen-carbonate by under the condition for structure auxiliary, successfully synthesize nano TiO 2 porous hollow sphere, and utilize the material analysis methods such as SEM, TEM, XDR and BET to characterize product.Result shows, products therefrom is anatase titanium dioxide, and sphere diameter and wall thickness are about 100nm, 20nm respectively, and pattern is even, better dispersed.Obtained TiO
2hollow ball sample has extremely strong adsorptivity to organic dye, and can be sharp sense formaldehyde gas, there is good air-sensitive performance.
Embodiment 1
A preparation method for nanometer porous titanium dioxide hollow ball, specifically implements according to the following steps:
Step 1, adds 1.5ml tetrabutyl titanate in 10ml dehydrated alcohol, after mixing, instills in 50ml deionized water under magnetic agitation, and hydrolysis generates oyster white TiO 2 sol, continues stirring 20 ~ 30min;
Step 2, by the TiO 2 sol washes of absolute alcohol generated in step 1, puts into tetrafluoroethylene water heating kettle liner, adds 74ml dehydrated alcohol and 1g bicarbonate of ammonia, stir.Liner containing above-mentioned mixing solutions is placed in stainless steel outer sleeve obturage, puts into baking oven, take out after constant temperature 180 DEG C heating 45h and naturally cool to room temperature.
Step 3, opens kettle cover, removing supernatant liquid, through collected after centrifugation bottoms, then use deionized water and absolute ethanol washing hydrothermal product respectively by ultrasonic, centrifugal, finally product is placed in 60 DEG C of dry 6h of baking oven, namely obtains nanometer porous titanium dioxide hollow ball.
Embodiment 2
A preparation method for nanometer porous titanium dioxide hollow ball, specifically implements according to the following steps:
Step 1, adds 2ml tetrabutyl titanate in 10ml dehydrated alcohol, after mixing, instills in 50ml deionized water under magnetic agitation, and hydrolysis generates oyster white TiO 2 sol, continues stirring 20 ~ 30min;
Step 2, by the TiO 2 sol washes of absolute alcohol generated in step 1, puts into tetrafluoroethylene water heating kettle liner, adds 72ml dehydrated alcohol and 1.5g bicarbonate of ammonia, stir.Liner containing above-mentioned mixing solutions is placed in stainless steel outer sleeve obturage, puts into baking oven, take out after constant temperature 180 DEG C heating 45h and naturally cool to room temperature.
Step 3, opens kettle cover, removing supernatant liquid, through collected after centrifugation bottoms, then use deionized water and absolute ethanol washing hydrothermal product respectively by ultrasonic, centrifugal, finally product is placed in 60 DEG C of dry 6h of baking oven, namely obtains nanometer porous titanium dioxide hollow ball.
Embodiment 3
A preparation method for nanometer porous titanium dioxide hollow ball, specifically implements according to the following steps:
Step 1, adds 2.5ml tetrabutyl titanate in 10ml dehydrated alcohol, after mixing, instills in 50ml deionized water under magnetic agitation, and hydrolysis generates oyster white TiO 2 sol, continues stirring 20 ~ 30min;
Step 2, by the TiO 2 sol washes of absolute alcohol generated in step 1, puts into tetrafluoroethylene water heating kettle liner, adds 70ml dehydrated alcohol and 2.2g bicarbonate of ammonia, stir.Liner containing above-mentioned mixing solutions is placed in stainless steel outer sleeve obturage, puts into baking oven, take out after constant temperature 180 DEG C heating 45h and naturally cool to room temperature.
Step 3, opens kettle cover, removing supernatant liquid, through collected after centrifugation bottoms, then use deionized water and absolute ethanol washing hydrothermal product respectively by ultrasonic, centrifugal, finally product is placed in 60 DEG C of dry 6h of baking oven, namely obtains nanometer porous titanium dioxide hollow ball.
Claims (5)
1. a preparation method for nanometer porous titanium dioxide hollow ball, specifically implements according to the following steps:
Step 1,3 ~ 5:20:100 measures tetrabutyl titanate, dehydrated alcohol and deionized water by volume, adds in dehydrated alcohol by the tetrabutyl titanate measured, after mixing, instill under magnetic agitation in deionized water, hydrolysis generates oyster white TiO 2 sol, continues stirring 20 ~ 30min;
Step 2, by the TiO 2 sol washes of absolute alcohol generated in step 1, puts into tetrafluoroethylene water heating kettle liner, adds dehydrated alcohol and structure directing agent, stirs; Liner containing above-mentioned mixing solutions is placed in stainless steel outer sleeve obturage, puts into baking oven, take out after thermostatically heating certain hour and naturally cool to room temperature;
Step 3, opens kettle cover, removing supernatant liquid, through collected after centrifugation bottoms, then use deionized water and absolute ethanol washing hydrothermal product respectively by ultrasonic, centrifugal, finally product is placed in the dry 6h of baking oven, namely obtains nanometer porous titanium dioxide hollow ball.
2. the preparation method of a kind of nanometer porous titanium dioxide hollow ball according to claim 1, is characterized in that, the addition of dehydrated alcohol described in step 2 is make mixed solution total amount reach 70% ~ 75% of tetrafluoroethylene water heating kettle total volume.
3. the preparation method of a kind of nanometer porous titanium dioxide hollow ball according to claim 1, is characterized in that, structure directing agent described in step 2 is bicarbonate of ammonia, bicarbonate of ammonia and TiO 2 sol mass ratio 20 ~ 25:7.
4. the preparation method of a kind of nanometer porous titanium dioxide hollow ball according to claim 1, is characterized in that, Heating temperature described in step 2 is 180 DEG C, and heat-up time is 45h ~ 48h.
5. the preparation method of a kind of nanometer porous titanium dioxide hollow ball according to claim 1, is characterized in that, time of drying described in step 3 is 60 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106830071A (en) * | 2017-03-09 | 2017-06-13 | 吉林大学 | A kind of preparation method of the spherical nano titanium oxide doped with rare earth |
| CN108821334A (en) * | 2018-08-13 | 2018-11-16 | 河南师范大学 | A kind of method that hydro-thermal method synthesizes hollow prismatic titanium dioxide nano material |
| CN111640924A (en) * | 2020-06-05 | 2020-09-08 | 新昌县华发机械股份有限公司 | Shell-core structure porous carbon-TiO2Positive electrode material of lithium-sulfur battery and preparation method thereof |
| CN113773569A (en) * | 2021-11-02 | 2021-12-10 | 衢州市洁妮肤日用品有限责任公司 | Antibacterial bath ball and preparation method thereof |
| CN114263039A (en) * | 2022-02-17 | 2022-04-01 | 王进 | Drug-loaded slow-release coating repairing agent and preparation method thereof |
-
2014
- 2014-10-15 CN CN201410550111.XA patent/CN105565375A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106830071A (en) * | 2017-03-09 | 2017-06-13 | 吉林大学 | A kind of preparation method of the spherical nano titanium oxide doped with rare earth |
| CN108821334A (en) * | 2018-08-13 | 2018-11-16 | 河南师范大学 | A kind of method that hydro-thermal method synthesizes hollow prismatic titanium dioxide nano material |
| CN111640924A (en) * | 2020-06-05 | 2020-09-08 | 新昌县华发机械股份有限公司 | Shell-core structure porous carbon-TiO2Positive electrode material of lithium-sulfur battery and preparation method thereof |
| CN111640924B (en) * | 2020-06-05 | 2022-01-21 | 新昌县华发机械股份有限公司 | Shell-core structure porous carbon-TiO2Positive electrode material of lithium-sulfur battery and preparation method thereof |
| CN113773569A (en) * | 2021-11-02 | 2021-12-10 | 衢州市洁妮肤日用品有限责任公司 | Antibacterial bath ball and preparation method thereof |
| CN114263039A (en) * | 2022-02-17 | 2022-04-01 | 王进 | Drug-loaded slow-release coating repairing agent and preparation method thereof |
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Application publication date: 20160511 |