CN102895964A - Preparation method of blue flaky titanium dioxide nano material - Google Patents
Preparation method of blue flaky titanium dioxide nano material Download PDFInfo
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- CN102895964A CN102895964A CN2012103972720A CN201210397272A CN102895964A CN 102895964 A CN102895964 A CN 102895964A CN 2012103972720 A CN2012103972720 A CN 2012103972720A CN 201210397272 A CN201210397272 A CN 201210397272A CN 102895964 A CN102895964 A CN 102895964A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- 239000010936 titanium Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical group [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 4
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 28
- 238000010521 absorption reaction Methods 0.000 description 7
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 6
- 229960000907 methylthioninium chloride Drugs 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
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- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
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- 230000001276 controlling effect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical group [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
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- 238000006555 catalytic reaction Methods 0.000 description 1
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- 239000002537 cosmetic Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
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- -1 exists anatase Chemical compound 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
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- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 238000000593 microemulsion method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
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- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
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- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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Abstract
The invention relates to a preparation method of a blue flaky titanium dioxide nano material, which comprises the following specific steps: dispersing a titanium source in a solvent, adding a morphology control agent, and stirring to obtain a transparent solution; then transferring the transparent solution into a reaction kettle for reaction, naturally cooling, washing, centrifuging and drying to obtain a blue flaky titanium dioxide nano material; the material has the grain size of 10-30 nm, and the crystal form of anatase can absorb visible light of 400-700 nm. The blue flaky titanium dioxide nano material obtained by the invention has the characteristics that: wide raw material source, simple preparation method, controllable material color and adjustable shape. The material realizes the breakthrough of the titanium dioxide nano material from white to color again, and is expected to be applied to the sewage treatment industry.
Description
Technical field
The present invention relates to a kind of blue plate-like titanium dioxide preparations of nanomaterials method, belong to nano material and photocatalysis technology field.
Background technology
Titanium dioxide (TiO
2) be a kind of very important transition metal oxide, have that nontoxic, oxidability is strong, a good stability and the advantage such as can reuse and be widely used in the industries such as coating, paint, toothpaste and cosmetics.1972, the professor Fujishima of Tokyo Univ Japan found photodissociation water phenomenon at titanium dioxide electrodes, thereby had opened up this new field of conductor photocatalysis, had risen afterwards the research boom to titanium dioxide in the worldwide.The main method of synthesis of titanium dioxide has hydrothermal synthesis method, colloidal sol ~ gel method, solvent-thermal method, chemical gaseous phase deposition method and microemulsion method now.Than many synthetic methods, because solvent-thermal method has the advantages such as simple to operate, safe, that equipment requirement is low, and favored by scientific researchers.
Titanium dioxide mainly exists anatase, rutile and three kinds of crystal formations of brockite.In order to alleviate energy and environment problem of today, scientific researchers conduct extensive research anatase titanium dioxide in recent years, such as solar cell, photolysis water hydrogen and photocatalytic degradation.But because the band gap of anatase titanium dioxide is 3.2eV, can only absorb and only account for 5% ultraviolet light in the sunshine, can not take full advantage of solar energy, thereby need to carry out various modifications to it strengthens visible Optical Absorption, the color of while its material itself also can be changed into by white coloured, and the sample that mixes such as N is that the sample that pale yellow powder and H mix is black powder.At present main method of modifying has that noble metal loading, metal oxide are compound, metal and nonmetal doping and surface dye sensitization etc., has cooperative effect between them, effectively can greatly strengthen utilization to solar energy in conjunction with multiple modification.Wherein the above two mainly are by the right effective separation in promotion electronics ~ hole, improve the light quantum utilization rate, thereby strengthen the effective utilization to energy.But these two kinds of methods can not solve visible Optical Absorption at all, therefore need to its role is to change the position of valence band or conduction band in conjunction with afterwards both modifications, reduce band gap, thereby improve visible Optical Absorption.
Summary of the invention
To the objective of the invention is to take full advantage of solar energy in order strengthening visible Optical Absorption, thereby to alleviate world energy sources and environmental problem and a kind of blue plate-like titanium dioxide preparations of nanomaterials method is provided; Mainly by titanium dioxide is carried out modification, make its color become blueness by white, form simultaneously sheet-like morphology, thereby overcome titanium dioxide to visible absorption difficulty and the low problem of utilization rate.
Technical scheme of the present invention is: a kind of blue plate-like titanium dioxide preparations of nanomaterials method, and concrete steps are as follows: the titanium source is dispersed in the solvent, adds the pattern controlling agent again, stir to get clear solution; Then clear solution is moved to reaction kettle for reaction, natural cooling, washing, centrifugal, dry, at last blue plate-like titanium dioxide nano material; This material grains is of a size of 10 ~ 30nm, and crystal formation is Detitanium-ore-type, can absorb 400 ~ 700nm visible light.
Preferred titanium source is butyl titanate or isopropyl titanate; Preferred solvent is ethanol, propyl alcohol or butanols; Preferred pattern controlling agent is that mass concentration is 30% ~ 50% hydrofluoric acid; The volume ratio of preferred titanium source and solvent is 0.2 ~ 0.4:1; The volume ratio of preferred titanium source and pattern controlling agent is 4 ~ 20:1; Preferable reaction temperature is 100 ~ 200 ° of C; Reaction time is 12 ~ 60h.
The present invention is for the test of this material light catalysis property, and being chosen in the methylene blue solution of degrading under the visible light is probe reaction, and reactor selects Shanghai than the BI-GHX-V type photocatalysis instrument of bright Instr Ltd., and its light source is xenon lamp, and power is 500W.Concrete experimental procedure is as follows: add 50mg sample and 30ml5mg/L methylene blue solution in test tube, put into airtight Photoreactor, stir 1h, make it reach adsorption equilibrium.Open xenon lamp, shine, observing response liquid change color.Reaction 3h, wherein every the 1h sampling, centrifugal, ultraviolet-uisible spectrophotometer is measured Methylene Blue in Solution concentration, and result and commercial P25 compare.
Beneficial effect:
The present invention has overcome the many disadvantages of other synthetic methods by synthetic this blueness plate-like titanium dioxide nano material of solvent-thermal method, has the advantages such as simple to operate, safe, that equipment requirement is low.Realized simultaneously titanium dioxide nano material by white to coloured again breakthrough, the qualitative explanation has closely relation to Optical Absorption and itself material color.Simultaneously, grain morphology is carried out Effective Regulation, improved it to visible Optical Absorption and utilization rate.In addition, this material has excellent Photocatalytic Degradation Property, can be applied to sewage treatment industry.
Description of drawings
Fig. 1 is sample T
0XRD figure, illustration is dispersed in photo in the ethanol for it;
Fig. 2 is sample T
0SEM figure;
Fig. 3 is sample T
0TEM figure;
Fig. 4 is sample T
0Solid UV-Vis figure;
Fig. 5 is sample T
0The Photocatalytic Degradation Property comparison diagram;
Fig. 6 is sample T
1XRD figure, illustration is dispersed in photo in the ethanol for it;
Fig. 7 is sample T
1SEM figure;
Fig. 8 is sample T
2XRD figure, illustration is dispersed in photo in the ethanol for it;
Fig. 9 is sample T
2SEM figure.
The specific embodiment
Below by embodiment, further illustrate outstanding feature of the present invention and marked improvement, only be this patent is described and do not limit this patent.
[example 1]
Sample T
0Preparation: add respectively 100ml butanols and 20ml butyl titanate in plastic beaker, solution A stirs to get.Then in solution A, dropwise add 1.0ml50% hydrofluoric acid, stir to get settled solution B.Solution B is moved to reactor, under 180 ° of C, react 30h.Naturally cooling (blue precipitation), with ethanol washing and centrifugal 3 times, drying, at last blue sheet anatase titanium dioxide sample T
0In ethanol, it is dispersed in photo in the ethanol shown in the upper right illustration of Fig. 1, is blueness with sample dissolution; Sample T as can be known
0Be the anatase titanium dioxide (see figure 1), crystallite dimension is 16nm, and pattern is sheet (seeing Fig. 2-3), can absorb the visible light (see figure 4) of 400nm ~ 700nm.This sample T
0Under visible light, the methylene blue degradation rate is reached 95.1%, is better than commercial P25(75.3%) (see figure 5).
[example 2]
Sample T
1Preparation: add respectively 80ml propyl alcohol and 20ml isopropyl titanate in plastic beaker, solution A stirs to get.Then in solution A, dropwise add 3.6ml40% hydrofluoric acid, stir to get settled solution B.Solution B is moved to reactor, under 100 ° of C, react 12h.Naturally cooling (blue precipitation), with ethanol washing and centrifugal 3 times, drying, at last blue sheet anatase titanium dioxide sample T
1In ethanol, it is dispersed in photo in the ethanol shown in the upper right illustration of Fig. 6, is blueness with sample dissolution; Know sample T
1Be the anatase titanium dioxide (see figure 6), crystallite dimension is 14nm, and pattern is the sheet (see figure 7), can absorb the visible light of 400nm ~ 700nm.This sample T
1Under visible light, the methylene blue degradation rate is reached 96.7%, be better than commercial P25(74.6%).
[example 3]
Sample T
2Preparation: add respectively 50ml ethanol and 20ml butyl titanate in plastic beaker, solution A stirs to get.Then in solution A, dropwise add 5.0ml30% hydrofluoric acid, stir to get settled solution B.Solution B is moved to reactor, under 200 ° of C, react 60h.Naturally cooling (blue precipitation), with ethanol washing and centrifugal 3 times, drying, at last blue sheet anatase titanium dioxide sample T
2In ethanol, it is dispersed in photo in the ethanol shown in the upper right illustration of Fig. 8, is blueness with sample dissolution; Sample T as can be known
2Be the anatase titanium dioxide (see figure 8), crystallite dimension is 28nm, and pattern is the sheet (see figure 9), can absorb the visible light of 400nm ~ 700nm.This sample T
2Under visible light, the methylene blue degradation rate is reached 96.2%, be better than commercial P25(74.7%).
Claims (6)
1. blue plate-like titanium dioxide preparations of nanomaterials method, concrete steps are as follows: the titanium source is dispersed in the solvent, adds the pattern controlling agent again, stir to get clear solution; Then clear solution is moved to reaction kettle for reaction, natural cooling, washing, centrifugal, dry, at last blue plate-like titanium dioxide nano material; This material grains is of a size of 10 ~ 30nm, and crystal formation is Detitanium-ore-type, can absorb 400 ~ 700nm visible light.
2. preparation method according to claim 1 is characterized in that described titanium source is butyl titanate or isopropyl titanate.
3. preparation method according to claim 1 is characterized in that described solvent is ethanol, propyl alcohol or butanols.
4. preparation method according to claim 1 is characterized in that described pattern controlling agent is that mass concentration is 30% ~ 50% hydrofluoric acid.
5. preparation method according to claim 1, the volume ratio that it is characterized in that titanium source and solvent is 0.2 ~ 0.4:1; The volume ratio of titanium source and pattern controlling agent is 4 ~ 20:1.
6. preparation method according to claim 1 is characterized in that reaction temperature is 100 ~ 200 ° of C, and the reaction time is 12 ~ 60h.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553124A (en) * | 2013-11-08 | 2014-02-05 | 中国科学技术大学 | Method for preparing blue titanium dioxide |
| CN103657619A (en) * | 2013-10-16 | 2014-03-26 | 江苏大学 | Preparation method of titanium dioxide nanosheet photocatalytic material with controllable size |
| CN103657624A (en) * | 2013-12-10 | 2014-03-26 | 南京工业大学 | Gray nano titanium dioxide material and preparation method and application thereof |
| CN104724755A (en) * | 2015-03-06 | 2015-06-24 | 华北电力大学 | Preparation method of micron-sized lamellar titanium dioxide nano material |
| CN106397769A (en) * | 2016-08-29 | 2017-02-15 | 广东丹邦科技有限公司 | Polyimide and titanium dioxide nano-sheet composite film and making method thereof |
| CN106582595A (en) * | 2016-12-28 | 2017-04-26 | 上海应用技术大学 | Preparation method for blue TiO2 catalyst |
| CN107140684A (en) * | 2017-06-13 | 2017-09-08 | 重庆邮电大学 | A kind of preparation method of titanium dioxide macro nanometer piece and products thereof |
| CN107827152A (en) * | 2017-11-09 | 2018-03-23 | 中国科学院上海硅酸盐研究所 | Blue titanium dioxide for carbon dioxide photocatalysis synthesizing methane and preparation method thereof |
| CN109081372A (en) * | 2018-10-23 | 2018-12-25 | 亚士漆(上海)有限公司 | A kind of anatase-type nanometer titanium dioxide, and its preparation method and application |
| CN112028119A (en) * | 2020-09-09 | 2020-12-04 | 晋中学院 | Anatase TiO with co-exposed {101}, {100} and {111} -crystal faces2Nanocrystal |
| CN112591792A (en) * | 2020-12-30 | 2021-04-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Simple preparation method of colored titanium dioxide for photocatalysis |
| CN112850784A (en) * | 2021-02-26 | 2021-05-28 | 中国检验检疫科学研究院 | Synthetic method and application of flaky TiO nano material |
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| CN103657619A (en) * | 2013-10-16 | 2014-03-26 | 江苏大学 | Preparation method of titanium dioxide nanosheet photocatalytic material with controllable size |
| CN103657619B (en) * | 2013-10-16 | 2016-04-27 | 江苏大学 | The preparation method of the titanium dioxide nanosheet photocatalytic material that a kind of size is controlled |
| CN103553124B (en) * | 2013-11-08 | 2015-03-11 | 中国科学技术大学 | Method for preparing blue titanium dioxide |
| CN103553124A (en) * | 2013-11-08 | 2014-02-05 | 中国科学技术大学 | Method for preparing blue titanium dioxide |
| CN103657624A (en) * | 2013-12-10 | 2014-03-26 | 南京工业大学 | Gray nano titanium dioxide material and preparation method and application thereof |
| CN103657624B (en) * | 2013-12-10 | 2016-04-13 | 南京工业大学 | Gray nano titanium dioxide material and preparation method and application thereof |
| CN104724755A (en) * | 2015-03-06 | 2015-06-24 | 华北电力大学 | Preparation method of micron-sized lamellar titanium dioxide nano material |
| CN106397769B (en) * | 2016-08-29 | 2019-02-05 | 深圳丹邦科技股份有限公司 | A kind of polyimides titanium dioxide nanoplate laminated film and preparation method thereof |
| CN106397769A (en) * | 2016-08-29 | 2017-02-15 | 广东丹邦科技有限公司 | Polyimide and titanium dioxide nano-sheet composite film and making method thereof |
| CN106582595B (en) * | 2016-12-28 | 2019-07-23 | 上海应用技术大学 | A kind of blue TiO2The preparation method of catalyst |
| CN106582595A (en) * | 2016-12-28 | 2017-04-26 | 上海应用技术大学 | Preparation method for blue TiO2 catalyst |
| CN107140684A (en) * | 2017-06-13 | 2017-09-08 | 重庆邮电大学 | A kind of preparation method of titanium dioxide macro nanometer piece and products thereof |
| CN107140684B (en) * | 2017-06-13 | 2019-06-21 | 重庆邮电大学 | A kind of preparation method and products thereof of titanium dioxide macro nanometer piece |
| CN107827152A (en) * | 2017-11-09 | 2018-03-23 | 中国科学院上海硅酸盐研究所 | Blue titanium dioxide for carbon dioxide photocatalysis synthesizing methane and preparation method thereof |
| CN107827152B (en) * | 2017-11-09 | 2019-07-16 | 中国科学院上海硅酸盐研究所 | Blue titanium dioxide and preparation method thereof for carbon dioxide photocatalysis synthesizing methane |
| CN109081372A (en) * | 2018-10-23 | 2018-12-25 | 亚士漆(上海)有限公司 | A kind of anatase-type nanometer titanium dioxide, and its preparation method and application |
| CN112028119A (en) * | 2020-09-09 | 2020-12-04 | 晋中学院 | Anatase TiO with co-exposed {101}, {100} and {111} -crystal faces2Nanocrystal |
| CN112028119B (en) * | 2020-09-09 | 2022-10-11 | 晋中学院 | Anatase TiO with co-exposed {101}, {100} and {111} -crystal faces 2 Nanocrystal |
| CN112591792A (en) * | 2020-12-30 | 2021-04-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Simple preparation method of colored titanium dioxide for photocatalysis |
| CN112850784A (en) * | 2021-02-26 | 2021-05-28 | 中国检验检疫科学研究院 | Synthetic method and application of flaky TiO nano material |
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Application publication date: 20130130 |