CN102500349A - Flower-like titanium dioxide microsphere photocatalytic material and preparation method thereof - Google Patents
Flower-like titanium dioxide microsphere photocatalytic material and preparation method thereof Download PDFInfo
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- CN102500349A CN102500349A CN2011103052767A CN201110305276A CN102500349A CN 102500349 A CN102500349 A CN 102500349A CN 2011103052767 A CN2011103052767 A CN 2011103052767A CN 201110305276 A CN201110305276 A CN 201110305276A CN 102500349 A CN102500349 A CN 102500349A
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Abstract
The invention relates to flower-like titanium dioxide microsphere photocatalytic material and a preparation method thereof. The photocatalytic material is formed by double-pyramid shaped single crystals of titanium dioxide. The preparation method of the photocatalytic material comprises the following steps: (1) adding a titanium source into an aqueous solution system, adding hydrogen peroxide and hydrochloric acid which serve as the regulator for the hydrolysis of the titanium source and growth of the single crystals, and subjecting the materials to hydrothermal reaction at 120-220 DEG C for 3 to 36 hours to obtain flower-like titanium dioxide microspheres; (2) washing to remove other impurity ions in the solution by water washing centrifugation; and (3) drying samples by using a vacuum drying box to obtain the powder of the flower-like titanium dioxide microsphere photocatalytic material. The preparation method of the flower-like titanium dioxide microsphere photocatalytic material has the advantages of simple preparation process, mild condition and convenience of post-processing and is suitable for preparing the flower-like titanium dioxide microsphere photocatalytic material on a large scale.
Description
Technical field
The present invention relates to catalysis material of a kind of novel special appearance and preparation method thereof, belong to the photocatalysis technology field.
Background technology
Modern industry and rapid development of science and technology; On the one hand; Greatly enriched people's material and cultural life, promoted the civilization and progress of human society, the generation and the discharging that bring a large amount of hazardous contaminants again simultaneously; The discharging that particularly contains pollutants such as phenyl ring, heterocycle, halogenated compound and NOx, SOx in waste gas, the waste water is more and more; Destroyed human atmosphere, water source and soil environment of depending on for existence, had a strong impact on human normal life and production, even jeopardized human existence.At present, the degree of concern of the government department of countries in the world, research institution's environmental pollution problem has reached unprecedented height, and many countries have dropped into great amount of manpower and material resources are used for surrounding purifying material and environmental improvement Study on Technology and exploitation.
Japanese scholar Fujishima in 1972 and Honda are at n type semiconductor titanium dioxide (TiO
2) find the photoelectrocatalysis decomposing phenomenon of water on the monocrystalline electrode; S.N.Frank in 1976 etc. are used for catalysis photodissociation pollutant with semi-conducting material, have obtained breakthrough progress.Since then, semi-conductive photocatalytic effect and potential application thereof have caused people's very big interest and have obtained research widely.Nano titanium oxide has that photochemical properties is stable, non-secondary pollution and advantage such as cheap and easy to get, is considered to one of catalysis material of tool application prospect.Big quantity research shows that factors such as the catalytic activity of titanium dioxide and crystal phase structure, crystal face characteristic, degree of crystallinity and pattern are closely related.
In order to realize regulation and control to titanium dioxide crystal phase structure, crystal face characteristic, degree of crystallinity and pattern; People have done a lot of researchs; Have some research work to be conceived to the exploration of synthetic method, the wet chemical method of having developed at present mainly comprises preparation methods such as hydro-thermal method, solvent-thermal method, sol-gel process and solid precursor method.Also have the other research work to focus on that additive such as application surface activating agent controls the growth of crystal, the final regulation and control that realize crystal phase structure, crystal face characteristic and pattern.Single from pattern, there has been the titanium dioxide of multiple patterns such as ball, bar-shaped, tubulose, linear, octahedra, banded, thin slice to be produced out.
Yet up to the present, the flower-shaped microballoon of being made up of two pyramid titanium dioxide single crystallines does not also appear in the newspapers as yet.And, in the said method, the reaction temperature that the needs that have are very high, the product postprocessing that has is loaded down with trivial details, and is repeatable poor, is unfavorable for mass preparation.
Summary of the invention
The present invention adopts hydrogen peroxide solution and hydrochloric acid as conditioning agent, has obtained a kind of novel flower-shaped microballoon that is made up of two pyramid titanium dioxide single crystallines.The present invention is also to present specially-shaped titanium dioxide preparation method existence condition is harsh, process is complicated, the problem of poor repeatability, found that technology is simple, mild condition, the approach that can repeatedly repeat in a large number to prepare.
Specially-shaped titanium dioxide catalysis material of the present invention is made up of two pyramid titanium dioxide single crystallines.Said Preparation of catalysts method may further comprise the steps:
(1) adopts the Hydrothermal Preparation titanium dioxide microballoon sphere.Stir down, the titanium source is joined contain in finite concentration hydrogen peroxide solution and the aqueous solution of hydrochloric acid, after stirring, change over to and carry out hydro-thermal reaction in the agitated reactor, and control reaction temperature and reaction time.Through above method, can obtain flower-shaped titanium dioxide microballoon sphere.
(2) adopt secondary water to titanium dioxide microballoon sphere washing 3～8 times, remove unreacted raw material, accessory substance and other impurity.
(3) place 60 ℃ of vacuum drying chambers dry flower-shaped titanium dioxide microballoon sphere, obtain flower-shaped titanic oxide microsphere photocatalyst powder.
In the step (1), the optional titanium valve in described titanium source, titanium trichloride, titanium tetrachloride are preferably titanium trichloride.The concentration of hydrogen peroxide solution is 0.8～4.0mol/L, and the concentration of hydrochloric acid is 0.8～3.2mol/L; Hydrothermal temperature is 120～220 ℃, is preferably 180 ℃; The hydro-thermal time is 3～36 hours, is preferably 18 hours.
The present invention utilizes hydro-thermal method, can under the condition of gentleness, can prepare flower-shaped titanium dioxide microballoon sphere catalysis material fast in a large number.Compared with prior art, the present invention has advantages such as technology is simple, manufacturing cycle is short, reaction temperature is low, favorable repeatability.
The reaction of ultraviolet catalytic degraded methyl orange:
Under 20 ℃, be ultraviolet source with the high-pressure sodium lamp of 300W, in the 100mL quartz reactor, add 60mL methyl orange solution (20mg/L) and 0.06g catalyst; The distance of light source and quartz ampoule is 24cm, and dark reaction absorption 30 minutes makes dyestuff after catalyst surface reaches the adsorption-desorption balance; Begin to carry out light-catalyzed reaction; Took a sample once in per 0.5 hour, after the centrifugation, with its absorbance of UV-Vis spectrophotometric instrumentation.
Description of drawings
Fig. 1 is the scanning electron microscope diagram that embodiment 1 obtains product.
Fig. 2 embodiment 1 obtains the x-ray diffraction pattern of product.
The specific embodiment
Below in conjunction with instance the present invention is further detailed.
Embodiment 1
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 1.2mol/L and 1.6mol/L.Then, add 1.2 * 10 again
-4The mol titanium trichloride places autoclave with mixed liquor after stirring, and puts into 180 ℃ of baking ovens, reacts 18 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
The sem photograph of embodiment 1 products obtained therefrom is as shown in Figure 1, as can be seen from the figure, and the products obtained therefrom flower-shaped microballoon that the titanium dioxide single crystalline of two pyramid configurations is assembled into of serving as reasons.The X-ray crystallogram of embodiment 1 products obtained therefrom is as shown in Figure 2, and as can be seen from the figure, the standard diffracting spectrum (JCPDS:21-1272) of the diffraction maximum of products obtained therefrom and anatase phase titanium dioxide is in full accord.
Photocatalytic degradation methyl orange shows that the flower-shaped photocatalysis material of titanium dioxide of the present invention's preparation has photocatalytic activity preferably, and UV-irradiation is after 3 hours, and the methyl orange degradation rate reaches more than 80%.
Embodiment 2
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 1.6mol/L and 1.6mol/L.Then, add 1.2 * 10 again
-4The mol titanium trichloride places autoclave with mixed liquor after stirring, and puts into 180 ℃ of baking ovens, reacts 18 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
Embodiment 3
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 2.4mol/L and 1.6mol/L.Then, add 1.2 * 10 again
-4The mol titanium trichloride places autoclave with mixed liquor after stirring, and puts into 180 ℃ of baking ovens, reacts 18 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
Embodiment 4
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 1.2mol/L and 0.8mol/L.Then, add 1.2 * 10 again
-4The mol titanium trichloride places autoclave with mixed liquor after stirring, and puts into 180 ℃ of baking ovens, reacts 18 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
Embodiment 5
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 1.2mol/L and 2.4mol/L.Then, add 1.2 * 10 again
-4The mol titanium trichloride places autoclave with mixed liquor after stirring, and puts into 180 ℃ of baking ovens, reacts 18 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
Embodiment 6
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 1.2mol/L and 1.6mol/L.Then, add 1.2 * 10 again
-4The mol titanium trichloride places autoclave with mixed liquor after stirring, and puts into 180 ℃ of baking ovens, reacts 5 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
Embodiment 7
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 1.2mol/L and 1.6mol/L.Then, add 1.2 * 10 again
-4The mol titanium trichloride places autoclave with mixed liquor after stirring, and puts into 180 ℃ of baking ovens, reacts 10 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
Embodiment 8
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 1.2mol/L and 1.6mol/L.Then, add 1.2 * 10 again
-4The mol titanium trichloride places autoclave with mixed liquor after stirring, and puts into 180 ℃ of baking ovens, reacts 24 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
Embodiment 9
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 1.2mol/L and 1.6mol/L.Then, add 1.2 * 10 again
-4The mol titanium trichloride places autoclave with mixed liquor after stirring, and puts into 150 ℃ of baking ovens, reacts 18 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 1.2mol/L and 1.6mol/L.Then, add 1.2 * 10 again
-4The mol titanium trichloride places autoclave with mixed liquor after stirring, and puts into 200 ℃ of baking ovens, reacts 18 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
Embodiment 11
In the polytetrafluoroethyllining lining of agitated reactor, add secondary water, hydrogen peroxide solution and hydrochloric acid, make the concentration of hydrogen peroxide solution and hydrochloric acid be respectively 1.2mol/L and 1.6mol/L.Then, add 1.2 * 10 again
-4The mol titanium tetrachloride places autoclave with mixed liquor after stirring, and puts into 180 ℃ of baking ovens, reacts 18 hours.
Behind the question response still cool to room temperature, draw supernatant liquor and discard.With lower sediment with secondary water centrifuge washing 6 times.Washing is put into 60 ℃ of baking oven vacuum drying 12 hours with sediment after accomplishing, and obtains flower-shaped ball microballoon titanium dioxide optical catalyst.
Claims (8)
1. a flower-shaped titanium dioxide microballoon sphere catalysis material is characterized in that said catalyst is made up of the anatase phase titanium dioxide monocrystalline.
2. flower-shaped titanium dioxide microballoon sphere catalysis material according to claim 1 is characterized in that, said titanium dioxide single crystalline is two pyramid configurations.
3. the preparation method of the described flower-shaped titanium dioxide microballoon sphere catalysis material of claim 1 is characterized in that, this preparation method may further comprise the steps:
(1) adopts the flower-shaped titanium dioxide microballoon sphere of Hydrothermal Preparation.With 1.2 * 10
-4Mol titanium source joins to be contained in finite concentration hydrogen peroxide solution and the aqueous solution of hydrochloric acid, after stirring, changes over to and carries out hydro-thermal reaction in the agitated reactor, and the control reaction temperature in the reaction time, can make flower-shaped titanium dioxide microballoon sphere.
(2) adopt secondary water to titanium dioxide microballoon sphere washing 3～8 times, remove unreacted raw material, accessory substance and other impurity.
(3) place 60 ℃ of vacuum drying chambers dry flower-shaped titanium dioxide microballoon sphere, obtain flower-shaped titanic oxide microsphere photocatalyst powder.
4. the preparation method of flower-shaped titanium dioxide microballoon sphere catalysis material according to claim 3 is characterized in that, the optional titanium valve in employed titanium source, titanium trichloride, titanium tetrachloride are preferably titanium trichloride.
5. the preparation method of flower-shaped titanium dioxide microballoon sphere catalysis material according to claim 3 is characterized in that, the concentration of hydrogen peroxide solution is 0.8～4.0mol/L.
6. the preparation method of flower-shaped titanium dioxide microballoon sphere catalysis material according to claim 3 is characterized in that, the concentration of hydrochloric acid is 0.8～3.2mol/L.
7. the preparation method of flower-shaped titanium dioxide microballoon sphere catalysis material according to claim 3 is characterized in that, hydrothermal temperature is 120～220 ℃.
8. the preparation method of flower-shaped titanium dioxide microballoon sphere catalysis material according to claim 3 is characterized in that, in water-heat process, the hydro-thermal time is 3～36 hours, is preferably 18 hours.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102941076A (en) * | 2012-11-21 | 2013-02-27 | 华东理工大学 | {110} surface exposed titanium dioxide photocatalysis material and preparation method thereof |
| CN103285893A (en) * | 2013-06-26 | 2013-09-11 | 华东理工大学 | Method for preparing coralline porous silver bromiodide/silver photocatalyst |
| CN104810480A (en) * | 2015-04-22 | 2015-07-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for thin titanium dioxide layer of perovskite cell |
| CN105347394A (en) * | 2015-11-26 | 2016-02-24 | 黑龙江大学 | Method for synthesizing hierarchical-structure TiO2 microspheres by one-step hydrothermal method |
| CN106543775A (en) * | 2016-10-20 | 2017-03-29 | 上海江沪实业有限公司 | A kind of spandex fibre titanium dioxide and preparation method thereof |
| CN106590069A (en) * | 2016-11-29 | 2017-04-26 | 华东理工大学 | Self-cleaning hydrophobic titanium dioxide coating and preparation method thereof |
| CN106914230A (en) * | 2017-02-08 | 2017-07-04 | 武汉理工大学 | A kind of flower-shaped titania photocatalyst of helicoid and preparation method thereof |
| CN108249478A (en) * | 2018-01-30 | 2018-07-06 | 成都大学 | A kind of preparation method of micron of floral structure red schorl phase titanium dioxide |
| CN112758980A (en) * | 2019-11-06 | 2021-05-07 | 国家纳米科学中心 | TiO 22Nano material, preparation method and application thereof |
-
2011
- 2011-10-11 CN CN2011103052767A patent/CN102500349A/en active Pending
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102941076A (en) * | 2012-11-21 | 2013-02-27 | 华东理工大学 | {110} surface exposed titanium dioxide photocatalysis material and preparation method thereof |
| CN103285893A (en) * | 2013-06-26 | 2013-09-11 | 华东理工大学 | Method for preparing coralline porous silver bromiodide/silver photocatalyst |
| CN104810480A (en) * | 2015-04-22 | 2015-07-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for thin titanium dioxide layer of perovskite cell |
| CN105347394A (en) * | 2015-11-26 | 2016-02-24 | 黑龙江大学 | Method for synthesizing hierarchical-structure TiO2 microspheres by one-step hydrothermal method |
| CN106543775A (en) * | 2016-10-20 | 2017-03-29 | 上海江沪实业有限公司 | A kind of spandex fibre titanium dioxide and preparation method thereof |
| CN106590069A (en) * | 2016-11-29 | 2017-04-26 | 华东理工大学 | Self-cleaning hydrophobic titanium dioxide coating and preparation method thereof |
| CN106914230A (en) * | 2017-02-08 | 2017-07-04 | 武汉理工大学 | A kind of flower-shaped titania photocatalyst of helicoid and preparation method thereof |
| CN106914230B (en) * | 2017-02-08 | 2019-09-10 | 武汉理工大学 | A kind of flower-shaped titania photocatalyst of helicoid and preparation method thereof |
| CN108249478A (en) * | 2018-01-30 | 2018-07-06 | 成都大学 | A kind of preparation method of micron of floral structure red schorl phase titanium dioxide |
| CN108249478B (en) * | 2018-01-30 | 2020-03-17 | 成都大学 | Preparation method of rutile phase titanium dioxide with micro-flower structure |
| CN112758980A (en) * | 2019-11-06 | 2021-05-07 | 国家纳米科学中心 | TiO 22Nano material, preparation method and application thereof |
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