CN101955223A - Method for preparing nano-titanium dioxide powder - Google Patents
Method for preparing nano-titanium dioxide powder Download PDFInfo
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- CN101955223A CN101955223A CN 201010281484 CN201010281484A CN101955223A CN 101955223 A CN101955223 A CN 101955223A CN 201010281484 CN201010281484 CN 201010281484 CN 201010281484 A CN201010281484 A CN 201010281484A CN 101955223 A CN101955223 A CN 101955223A
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- 239000000843 powder Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 21
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 14
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 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 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 11
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 238000001816 cooling Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
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Abstract
The invention relates to a method for preparing nano-titanium dioxide powder, which comprises the following steps of: preparing a titanium dioxide hydrothermal reaction precursor; putting the prepared precursor into a reaction kettle, and putting the reaction kettle into a microwave hydrothermal synthesizer for reaction to obtain a reaction product; and washing and drying the obtained reaction product. The nano-titanium dioxide powder prepared by the method has the advantages of uniform particle size and high dispersibility.
Description
Technical field
The present invention relates to field of material preparation, relate in particular to a kind of preparation method of nano-titanium dioxide powder.
Background technology
TiO
2Be a kind of low price, be widely used, nontoxic, stable and inorganic materials that corrosion-resistant is good, be widely used in fields such as paint, coating, chemical fibre, plastics, pottery.Along with the development of nano material, nano-TiO
2Be widely used in catalyzer, sensor etc.Along with the technical progress and its good industrial prospect of dye sensitization solar battery in recent years, preferably select the nano-TiO of material as the light anode
2Powder also begins to obtain people and pays close attention to greatly.
In the prior art, TiO
2The preparation method of powder mainly contains high temperature solid-phase sintering method, sol-gel method and hydrothermal method.Wherein, be that " a kind of preparation method of nano titanium oxide " (patent No.: CN02145860.X) disclosed high temperature solid-phase sintering method need at high temperature be carried out, prepared TiO as denomination of invention
2Powder granularity is big, and sintering activity is low, and crystal grain is too grown up and reacted and is difficult for being difficult to obtain highly purified TiO fully
2Powder; Sol-gel method need be carried out later stage thermal treatment, makes powder hard aggregation occur, difficulties in dispersion; Hydrothermal synthesis method can carry out at a lower temperature, and gained powder dispersity and crystallinity are good, but preparation cycle is long, reaction process is wayward.
Summary of the invention
The present invention proposes a kind of preparation method of nano-titanium dioxide powder, the titanium dioxide powder epigranular, the favorable dispersity that obtain.
A kind of microwave hydrothermal prepares the method for nano-titanium dioxide powder, comprising:
Step 1: preparation titanium dioxide hydro-thermal reaction precursor;
Step 2: the precursor of step 1 preparation is placed reactor, and place the microwave hydrothermal synthesizer to react reactor, obtain reaction product;
Step 3: with the reaction product that step 2 obtains wash, drying.
Preferably, in the step 2, the described precursor liner of packing into is in the reactor of tetrafluoroethylene, and fixedly compactedness is 60%-80%, the fit sealing reactor.
Preferably, in the step 2, the temperature of reaction of microwave hydrothermal synthesizer is 160 ℃-200 ℃, and pressure is 1.0-2.5MPa, and the reaction times is 30-100min.
Preferably, in the step 1, tetrabutyl titanate and dehydrated alcohol are mixed, mixing back dropping distilled water, and after dripping end, stirring, obtain the hydro-thermal reaction precursor.
Preferably, in the step 1, the volume ratio of tetrabutyl titanate and dehydrated alcohol is 4: 1 to 6: 1.
Preferably, in the step 1, the amount that drips distilled water is 0.5-2ml, and the speed of dropping is 0.3-1ml/min.
Preferably, in the step 3, the reaction product washing sequence is that deionized water cleans repeatedly with dehydrated alcohol and cleans.
Preferably, in the step 3, when reaction product was dry, drying temperature was 100 ℃, and be 2-4 hour time of drying.
The beneficial effect that the present invention has:
The present invention proposes a kind of titanium dioxide powder preparation, carry out microwave hydrothermal synthesis of titanium dioxide powder, the titanium dioxide powder epigranular of preparation, favorable dispersity have crystallinity preferably.In addition, the present invention adopts hydro-thermal reaction and the synchronous technological process of microwave reaction, makes the production cycle shorten greatly, and save energy is enhanced productivity; Adopt the pressure-controlling reaction process, make reaction be subjected to ectocine little, TiO
2The preparation good reproducibility of powder.
Description of drawings
Fig. 1 is for adopting the TiO of the inventive method preparation
2Powder SEM figure spectrogram;
Fig. 2 is for adopting the TiO of the inventive method preparation
2Powder XRD figure spectrogram.
Embodiment
Embodiment one:
Step 1: preparation titanium dioxide hydro-thermal reaction precursor.Measure a certain amount of tetrabutyl titanate and dehydrated alcohol, the volume ratio of tetrabutyl titanate and dehydrated alcohol is 4: 1, magnetic agitation 0.5h mixes it, continue to drip 0.5ml distilled water then, the control rate of addition is 0.5ml/min, drips to finish back continuation stirring, obtains faint yellow colloidal sol, fully stir 1h again, promptly obtain the hydro-thermal reaction precursor.
Step 2: microwave-hydrothermal synthesis reaction.The precursor that step 1 the is obtained liner of packing into is in the reactor of tetrafluoroethylene, and fixedly compactedness is 70%, the fit sealing reactor.Reactor is placed microwave-assisted hydro-thermal synthesizer, and control reaction temperature is 180 ℃, and pressure is 1.0MPa, and the reaction times is 90min, reaches to be cooled to room temperature in the naturally cooling mode after the required time reaction finishes.
Step 3: washing, drying.The product that step 2 is obtained cleans repeatedly with deionized water earlier, adopts dehydrated alcohol to clean then 4 times, places 100 ℃ of dry 2h of loft drier, obtains nano titanium oxide white powder.
By implementing the titanium dioxide powder preparation that the present invention proposes, because microwave has quickened reaction process in hydrothermal reaction process, it is lower to have temperature of reaction, the advantage that the reaction times is shorter.Simultaneously, microwave has the microwave catalysis effect, can effectively promote reaction and improve the nano-powder quality.
As shown in Figure 1, adopt the TiO of the inventive method preparation
2The powder granule degree is evenly distributed, and good dispersion, no agglomeration.As shown in Figure 2, for adopting the TiO of the inventive method preparation
2Powder, it has good crystallinity.
Embodiment two:
Step 1: preparation titanium dioxide hydro-thermal reaction precursor.Measure a certain amount of tetrabutyl titanate and dehydrated alcohol, the volume ratio of tetrabutyl titanate and dehydrated alcohol is 5: 1, and magnetic agitation 1h mixes it.Continue then to drip 1ml distilled water, the control rate of addition is 0.5ml/min, drips the end back and continues to stir, and obtains faint yellow colloidal sol, fully stirs 0.5h again, promptly obtains the hydro-thermal reaction precursor.
Step 2: microwave-hydrothermal synthesis reaction.The precursor that step 1 the is obtained liner of packing into is in the reactor of tetrafluoroethylene, and fixedly compactedness is 80%, the fit sealing reactor.Reactor is placed microwave-assisted hydro-thermal synthesizer, and control reaction temperature is 200 ℃, and pressure is 1.5MPa, and the reaction times is 60min, reaches to be cooled to room temperature in the naturally cooling mode after the required time reaction finishes.
Step 3: washing, drying.The product that step 2 is obtained cleans repeatedly with deionized water earlier, adopts dehydrated alcohol to clean then 3 times, places 100 ℃ of dry 3h of loft drier, obtains nano titanium oxide white powder.
Embodiment three:
Step 1: preparation titanium dioxide hydro-thermal reaction precursor.Measure a certain amount of tetrabutyl titanate and dehydrated alcohol, the volume ratio of tetrabutyl titanate and dehydrated alcohol is 6: 1, continues then to drip 2ml distilled water, and the control rate of addition is 1ml/min, drips the end back and continues to stir, and obtains faint yellow colloidal sol.Fully stir 1h again, promptly obtain the hydro-thermal reaction precursor.
Step 2: microwave-hydrothermal synthesis reaction.The precursor that step 1 the is obtained liner of packing into is in the reactor of tetrafluoroethylene, and fixedly compactedness is 60%, the fit sealing reactor.Reactor is placed microwave-assisted hydro-thermal synthesizer, and control reaction temperature is 170 ℃, and pressure is 2.0MPa, and the reaction times is 40min, reaches to be cooled to room temperature in the naturally cooling mode after the required time reaction finishes.
Step 3: washing, drying.The product that step 2 is obtained cleans repeatedly with deionized water earlier, adopts dehydrated alcohol to clean then 3 times, places 100 ℃ of dry 4h of loft drier, obtains nano titanium oxide white powder.
The titanium dioxide powder preparation that the application of the invention provides carries out microwave hydrothermal synthesis of titanium dioxide powder, and the titanium dioxide powder epigranular of preparation, favorable dispersity have crystallinity preferably.In addition, the present invention adopts hydro-thermal reaction and the synchronous technological process of microwave reaction, makes the production cycle shorten greatly, and save energy is enhanced productivity; Adopt the pressure-controlling reaction process, make reaction be subjected to ectocine little, TiO
2The preparation good reproducibility of powder.
The above only is preferred embodiment of the present invention, and is in order to restriction the present invention, within the spirit and principles in the present invention not all, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. the preparation method of a nano-titanium dioxide powder is characterized in that, comprising:
Step 1: preparation titanium dioxide hydro-thermal reaction precursor;
Step 2: the precursor of step 1 preparation is placed reactor, and place the microwave hydrothermal synthesizer to react reactor, obtain reaction product;
Step 3: with the reaction product that step 2 obtains wash, drying.
2. method according to claim 1 is characterized in that:
In the step 2, the described precursor liner of packing into is in the reactor of tetrafluoroethylene, and fixedly compactedness is 60%-80%, the fit sealing reactor.
3. method according to claim 2 is characterized in that:
In the step 2, the temperature of reaction of microwave hydrothermal synthesizer is 160 ℃-200 ℃, and pressure is 1.0-2.5MPa, and the reaction times is 30-100min.
4. method according to claim 1 is characterized in that:
In the step 1, tetrabutyl titanate and dehydrated alcohol are mixed, mixing back dropping distilled water, and after dripping end, stirring, obtain the hydro-thermal reaction precursor.
5. method according to claim 4 is characterized in that:
In the step 1, the volume ratio of tetrabutyl titanate and dehydrated alcohol is 4: 1 to 6: 1.
6. method according to claim 5 is characterized in that:
In the step 1, the amount that drips distilled water is 0.5-2ml, and the speed of dropping is 0.3-1ml/min.
7. method according to claim 1 is characterized in that:
In the step 3, the reaction product washing sequence is that deionized water cleans repeatedly with dehydrated alcohol and cleans.
8. method according to claim 7 is characterized in that: in the step 3, when reaction product was dry, drying temperature was 100 ℃, and be 2-4 hour time of drying.
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| CN 201010281484 CN101955223A (en) | 2010-09-15 | 2010-09-15 | Method for preparing nano-titanium dioxide powder |
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|---|---|---|---|
| CN 201010281484 CN101955223A (en) | 2010-09-15 | 2010-09-15 | Method for preparing nano-titanium dioxide powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102800482A (en) * | 2012-08-07 | 2012-11-28 | 奇瑞汽车股份有限公司 | Method for preparing photoanode, photoanode, and dye-sensitized solar cell |
| CN103236535A (en) * | 2013-05-06 | 2013-08-07 | 武汉工程大学 | Titanium dioxide nano particle anode material of lithium ion power battery and method for preparing titanium dioxide nano particle anode material |
| WO2013139174A1 (en) * | 2012-03-19 | 2013-09-26 | The Hong Kong University Of Science And Technology | Incorporating metals, metal oxides and compounds on the inner and outer surfaces of nanotubes and between the walls of the nanotubes and preparation thereof |
| CN103641163A (en) * | 2013-11-28 | 2014-03-19 | 武汉大学 | Preparation method of nano TiO2 powder and method for preparing oxygen gas indicator from nano TiO2 powder |
| CN104609467A (en) * | 2015-01-21 | 2015-05-13 | 武汉理工大学 | Photoinduced red-turning titanium oxide as well as preparation method and application thereof |
-
2010
- 2010-09-15 CN CN 201010281484 patent/CN101955223A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 《化学通报》 20051231 白波 等 纳米TiO2的微波水热法制备及其光催化性能研究 776-780 1-7 , 第10期 * |
| 《环境科学与技术》 20090331 韦庆婷 等 纳米TiO2的溶胶－微波法合成及其光催化性能研究 第1-4页 1-8 第32卷, 第3期 * |
| 《环境科学与技术》 20090331 韦庆婷 等 纳米TiO2的溶胶－微波法合成及其光催化性能研究 第1-4页 1-8 第32卷, 第3期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013139174A1 (en) * | 2012-03-19 | 2013-09-26 | The Hong Kong University Of Science And Technology | Incorporating metals, metal oxides and compounds on the inner and outer surfaces of nanotubes and between the walls of the nanotubes and preparation thereof |
| US10238762B2 (en) | 2012-03-19 | 2019-03-26 | The Hong Kong University Of Science And Technology | Incorporating metals, metal oxides and compounds on the inner and outer surfaces of nanotubes and between the walls of the nanotubes and preparation thereof |
| CN102800482A (en) * | 2012-08-07 | 2012-11-28 | 奇瑞汽车股份有限公司 | Method for preparing photoanode, photoanode, and dye-sensitized solar cell |
| CN103236535A (en) * | 2013-05-06 | 2013-08-07 | 武汉工程大学 | Titanium dioxide nano particle anode material of lithium ion power battery and method for preparing titanium dioxide nano particle anode material |
| CN103641163A (en) * | 2013-11-28 | 2014-03-19 | 武汉大学 | Preparation method of nano TiO2 powder and method for preparing oxygen gas indicator from nano TiO2 powder |
| CN103641163B (en) * | 2013-11-28 | 2015-07-15 | 武汉大学 | Preparation method of nano TiO2 powder and method for preparing oxygen gas indicator from nano TiO2 powder |
| CN104609467A (en) * | 2015-01-21 | 2015-05-13 | 武汉理工大学 | Photoinduced red-turning titanium oxide as well as preparation method and application thereof |
| CN104609467B (en) * | 2015-01-21 | 2016-09-14 | 武汉理工大学 | A kind of light-induced variable red oxidization titanium and its preparation method and application |
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Application publication date: 20110126 |