CN102515271A - TiO2 powder with visible light catalytic activity and preparation method thereof - Google Patents
TiO2 powder with visible light catalytic activity and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of material science and specifically relates to a TiO2 powder with visible light catalytic activity and a preparation method thereof. The TiO2 powder of the invention contains crystal phases of: 90-100 wt% of anatase (TiO2), and 0-10 wt% of rutile (TiO2). The preparation process comprises main points of: preparing a forerunner liquid A from tetra-n-butyl titanate, absolute ethyl alcohol and glacial acetic acid; preparing secondary distilled water and absolute ethyl alcohol into a solution; adding hydrochloric acid and adjusting a pH value to 1-5; preparing a dropping solution B; adding the dropping solution B into the forerunner liquid A; carrying out isothermal stirring in a water-bath; carrying out stewing for a while, drying, grinding and calcining to obtain the TiO2 powder with high photocatalytic activity. The TiO2 powder of the invention has strong light absorption and photoresponse in wide spectrum scope namely under ultraviolet light and visible light irradiation and has visible light catalytic activity; and the method has advantages of simple preparation technology, low-cost equipment and easily controlled reaction process.
Description
Technical field
The invention belongs to material science, be specifically related to a kind of TiO with visible light catalysis activity
2Powder and preparation method thereof.
Background technology
TiO
2It is a kind of critical function material with broad prospect of application; Have unique function such as good photocatalytic activity, erosion resistance, intensive ultraviolet screening ability and electrochromism, be widely used in fields such as water resources protection, coating and automotive industry, transmitter and photochemical catalysis in recent years.TiO
2Can be as photocatalyst treatment sewage, under the uviolizing condition, the organic cpds of more than the 3000 kind of difficult degradation of can degrading.China is the raising of industrialization degree in recent decades; Caused increasing the weight of of water pollution, brought very big threat for ecotope and even people's health, country has also strengthened the input of anti-soil when formulating pollution exhaust criteria; Developing effectively, water pollution treatment technology can not be ignored TiO
2The technology of photocatalysis treatment sewage is with a wide range of applications at sewage treatment area.
At present, preparation TiO
2The method of powder mainly contains: liquid phase deposition, chemical Vapor deposition process and magnetron sputtering method etc., but the TiO that utilizes these methods to prepare
2Photocatalyst only has photocatalytic activity preferably under UV-light, and under visible light unglazed basically catalytic effect, and the equipment of these methods and complex process, the required temperature of technology is higher, the TiO for preparing
2The purity of powder is not high, and is dispersed bad.
Summary of the invention
The objective of the invention is problem, a kind of TiO with visible light catalysis activity is provided to the prior art existence
2Powder and preparation method thereof, TiO of the present invention
2Powder promptly all has stronger photoabsorption and photoresponse under UV-light and visible light radiation in the wide spectrum scope, be a kind of TiO with certain visible light catalysis activity
2Powder, preparation technology is simple, cheap device, and reaction process is controlled easily.
TiO with visible light catalysis activity of the present invention
2The crystalline phase of powder consists of, by weight percentage, and Detitanium-ore-type TiO
2: 90-100wt%, rutile TiO
2: 0-10wt%.
The present invention's preparation has the TiO of visible light catalysis activity
2The technical scheme of powder is carried out according to following steps:
(1) preparation precursor liquid A: the 5-25ml tetra-n-butyl titanate is added drop-wise in the 10-35ml absolute ethyl alcohol while stirring, splashes into the 1-10ml Glacial acetic acid min. 99.5 again, through the stirring of 20-50min, the yellow solution that obtains homogeneous transparent is precursor liquid A;
(2) preparation dropping liquid B: with 5-20ml redistilled water and 5-15ml absolute ethyl alcohol wiring solution-forming, add hydrochloride adjusted solution pH value, stir 10-30min, obtain the dropping liquid B of pH value for 1-5;
(3) preparation TiO
2Wet colloidal sol: dropping liquid B is added drop-wise among the precursor liquid A, in water-bath, after 50-70 ℃ of constant temperature stirs 2h-4h, obtains the faint yellow TiO of homogeneous transparent
2Wet colloidal sol leaves standstill after 15 hours subsequent use;
(4) preparation TiO
2Xerogel: with the TiO that obtains
2Wet colloidal sol in 50-80 ℃ of dry 24-72h, obtains TiO in vacuum drying oven
2Xerogel;
(5) preparation TiO
2Powder: with TiO
2After xerogel ground, in 400-600 ℃ of calcining 2-5h, temperature rise rate was 5-10 ℃/min under oxidizing atmosphere and normal pressure, to calcining and be cooled to the TiO that obtains after the room temperature
2Powder grinds, and promptly obtains to have the TiO of visible light catalysis activity
2Powder.
Wherein the stirring velocity described in step (1), (2) and (3) is 200-300r/min.
Rate of addition described in the step (1) is controlled by peristaltic pump, and its numerical value is 0.7-1ml/min.
Rate of addition described in the step (3) is controlled by peristaltic pump, and its numerical value is 0.1-0.4ml/min.
Concentration of hydrochloric acid described in the step (2) is 0.1-12 mol/l.
Compared with prior art, characteristics of the present invention and beneficial effect are:
TiO with photocatalytic activity provided by the present invention
2Powder is raw material with the tetra-n-butyl titanate, and reactant uniform mixing and reacting under liquid phase generates the stable sols system; Change gel into through placement for some time, because of the generation of gel, the immobilization of structure between particle in the gel; Also can effectively suppress particulate growth and aggregation procedure, thereby powder granularity is thin and monodispersity is little, at colloidal sol or gel state compacted under; Be lower than calcining formation oxide compound under traditional firing temperature, technology is easy, and preparation cost is lower; Be fit to suitability for industrialized production, have good social benefit and economic benefit.
Evaluation TiO provided by the present invention
2In the method for powder photocatalytic activity, do not adjust the pH value of organic pollutant, so just suppressed dark attitude absorption TiO
2The influence of powder photocatalytic activity it is generally acknowledged, pollutent is easy to absorption under the acidic conditions, causes TiO
2Powder photochemical catalysis effect enlarges markedly, and makes evaluation result depart from truth; And do not adjust pollutent pH value among the present invention, thereby institute's value is more truly described prepared TiO
2Powder photochemical catalysis effect.
Marked improvement of the present invention is the TiO for preparing
2Powder under ultraviolet source and visible light source, promptly all has stronger photoabsorption and photoresponse under the optical excitation of wavelength region 250-600nm, thereby has significantly improved TiO respectively
2Photocatalytic activity, can utilize visible light sources such as sunshine, effective organic and inorganic pollutant in the photodegradation water, and have higher effciency of energy transfer is for the practical application of sunlight catalytic degradation of contaminant provides platform.
Description of drawings
Fig. 1 is the TiO of the embodiment of the invention 1
2The X ray diffracting spectrum of powder product is among the figure
▲Represent Detitanium-ore-type TiO
2, its content is 100wt%;
Fig. 2 is the TiO of the embodiment of the invention 2
2The X ray diffracting spectrum of powder light product is among the figure
▲Represent Detitanium-ore-type TiO
2, ▼ represents rutile TiO
2, each crystal content is: Detitanium-ore-type 91wt%, rutile-type 9wt%.
Embodiment
Below in conjunction with concrete embodiment technical scheme of the present invention is described further:
The tetra-n-butyl titanate that the embodiment of the invention is selected for use, absolute ethyl alcohol, Glacial acetic acid min. 99.5 and hydrochloric acid are the pure level of general analysis;
The zero(ppm) water that the embodiment of the invention is selected for use is redistilled water;
The controlled liq flow device that adopts in the embodiment of the invention is a BT100-2J type peristaltic pump;
The drying plant that adopts in the embodiment of the invention is a QLF-6050 type vacuum drying oven;
The roasting apparatus that adopts in the embodiment of the invention is a DC-B type retort furnace;
The photocatalysis performance valuator device that adopts in the embodiment of the invention is that the many test tubes of XPA-7 type stir the photochemical reaction appearance;
Be adopted as UV-2550 type ultraviolet-visible pectrophotometer in the embodiment of the invention, analyze the methyl orange solution concentration change;
Adopt X'PertHighScorePlus software in the embodiment of the invention, the crystal phase structure of analytic sample also utilizes the crystal content of semi-quantitative analysis method analytic sample, and analytical instrument is a D/max-2550PC type polycrystalline X-ray diffractometer.
Embodiment 1
(1) preparation precursor liquid A: the 5ml tetra-n-butyl titanate is added drop-wise to while stirring in the absolute ethyl alcohol of 20ml, splashes into the 3ml Glacial acetic acid min. 99.5 again, through the stirring of 20min, the yellow solution that obtains homogeneous transparent is precursor liquid A;
(2) preparation dropping liquid B: with the solution that 5ml redistilled water and 10ml absolute ethyl alcohol are made into, use hydrochloride adjusted solution pH=2, stirring 20min obtains dropping liquid B;
(3) preparation TiO
2Wet colloidal sol: dropping liquid B is added drop-wise among the precursor liquid A, after 50 ℃ of constant temperature of water-bath stir 4h, obtains the faint yellow TiO of homogeneous transparent
2Wet colloidal sol leaves standstill after 15 hours subsequent use;
(4) preparation TiO
2Xerogel: with TiO
2Wet colloidal sol in 60 ℃ of dry 72h, obtains TiO in vacuum drying oven
2Xerogel;
(5) preparation TiO
2Powder: with TiO
2After xerogel ground, in 400 ℃ of calcining 3h, temperature rise rate was 5 ℃/min under oxidizing atmosphere and normal pressure, to the above-mentioned TiO that after calcining and activating, cooling, obtains
2Powder grinds, and promptly obtains to have the TiO of photocatalytic activity
2Powder.
Wherein said stirring velocity is 200r/min, and rate of addition is 0.7ml/min in the step (1), and rate of addition is 0.1ml/min in the step (3).
The method of the photocatalytic activity of evaluate catalysts sample is: the catalyzer that takes by weighing 0.015g adds 50ml and contains in the reservoir of methyl orange solution (mass concentration is 10mg/l); Keep catalyst reactor through magnetic agitation and be in suspended state, make reaction solution in reservoir and reactor drum, circulate through peristaltic pump.In the light-catalyzed reaction process, be radiation source with mercury lamp and Metal-halogen lamp respectively, every at a distance from the 5min sampling.Sample through centrifugal, filter after, measure its absorbance, and convert based on calibration curve and to become corresponding concentration.The catalytic activity of catalyzer is estimated through measuring the tropeolin-D percent of decolourization.Calculation formula is:
C' in the formula
0For reaching concentration after the adsorption equilibrium as the starting point concentration of light-catalyzed reaction; C
tBe the concentration of tropeolin-D in the t moment reaction liquid, η is the tropeolin-D percent of decolourization.The tropeolin-D percent of decolourization is high more, then explanation, and under mercury lamp or Metal-halogen lamp irradiation, the TiO of preparation
2The powder photocatalytic activity is high more, is easy to degradation of contaminant more.
Estimate TiO
2The method of powder crystal phase structure and crystal content is: adopt the crystal phase structure of X'PertHighScorePlus software analysis sample and utilize the crystal content of semi-quantitative analysis method analytic sample.
The TiO of preparation
2Each crystal content of powder is: Detitanium-ore-type 100wt%
With the mercury lamp is light source, and radiation 10min, its degradation rate are 92%; With the Metal-halogen lamp is light source, and radiation 10min, its degradation rate are 35%.
Embodiment 2
(1) with the 10ml tetra-n-butyl titanate in the absolute ethyl alcohol that is added drop-wise to 12ml while stirring, splash into the 7ml Glacial acetic acid min. 99.5 again, through the stirring of 30min, the yellow solution that obtains homogeneous transparent is precursor liquid A;
(2) preparation dropping liquid B: with 10ml redistilled water and 8ml absolute ethyl alcohol wiring solution-forming, use hydrochloride adjusted solution pH=2, stir 20min, obtain dropping liquid B;
(3) preparation TiO
2Wet colloidal sol: dropping liquid B is added drop-wise among the step precursor liquid A, behind 70 ℃ of stirrings of constant temperature water bath 2h, obtains the faint yellow TiO of homogeneous transparent
2Wet colloidal sol leaves standstill after 15 hours subsequent use;
(4) preparation TiO
2Xerogel: with TiO
2Wet colloidal sol in 70 ℃ of dry 60h, obtains TiO in vacuum drying oven
2Xerogel;
(5) preparation TiO
2Powder: with TiO
2After xerogel ground, in 500 ℃ of calcining 4h, temperature rise rate was 10 ℃/min under oxidizing atmosphere and normal pressure, to the above-mentioned TiO that after calcining and activating and cooling, obtains
2Powder grinds, and promptly obtains to have the TiO of photocatalytic activity
2Powder.
Wherein said stirring velocity is 250r/min, and rate of addition is 0.8ml/min in the step (1), and rate of addition is 0.2ml/min in the step (3).
The TiO of preparation
2Each crystal content of powder is: anatase octahedrite 91wt%, rutile 9wt%
With the mercury lamp is light source, and radiation 10min, its degradation rate are 96%; With the Metal-halogen lamp is light source, and radiation 10min, its degradation rate are 39%.
Embodiment 3
(1) preparation precursor liquid A: the 15ml tetra-n-butyl titanate is added drop-wise to while stirring in the absolute ethyl alcohol of 12ml, splashes into the 3ml Glacial acetic acid min. 99.5 again, through the stirring of 50min, the yellow solution that obtains homogeneous transparent is precursor liquid A;
(2) preparation dropping liquid B: with 20ml redistilled water and 8ml absolute ethyl alcohol wiring solution-forming, use hydrochloride adjusted solution pH=3, restir 30min obtains dropping liquid B;
(3) preparation TiO
2Wet colloidal sol: dropping liquid B is added drop-wise among the precursor liquid A, behind 60 ℃ of stirrings of constant temperature water bath 3h, obtains the faint yellow TiO of homogeneous transparent
2Wet colloidal sol leaves standstill after 15 hours subsequent use;
(4) preparation TiO
2Xerogel: with TiO
2Wet colloidal sol in 80 ℃ of dry 24h, obtains TiO in vacuum drying oven
2Xerogel;
(5) preparation TiO
2Powder: with TiO
2After xerogel ground, in 600 ℃ of calcining 2h, temperature rise rate was 10 ℃/min under oxidizing atmosphere and normal pressure, to the TiO that obtains after above-mentioned calcining and activating and the cooling
2Powder grinds, and promptly obtains to have the TiO of photocatalytic activity
2Powder.
Wherein said stirring velocity is 300r/min, and rate of addition is 0.9ml/min in the step (1), and rate of addition is 0.3ml/min in the step (3).
The TiO of preparation
2Each crystal content of powder is: anatase octahedrite 93wt%, rutile 7wt%
With the mercury lamp is light source, and radiation 10min, its degradation rate are 98%; With the Metal-halogen lamp is light source, and radiation 10min, its degradation rate are 10%.
Embodiment 4
(1) preparation precursor liquid A: the 25ml tetra-n-butyl titanate is added drop-wise to while stirring in the absolute ethyl alcohol of 35ml, splashes into the 5ml Glacial acetic acid min. 99.5 again, through the stirring of 50min, the yellow solution that obtains homogeneous transparent is precursor liquid A;
(2) preparation dropping liquid B: with 5ml redistilled water and 15ml absolute ethyl alcohol wiring solution-forming, use hydrochloride adjusted solution pH=5, restir 30min obtains dropping liquid B;
(3) preparation TiO
2Wet colloidal sol: dropping liquid B is added drop-wise among the precursor liquid A, behind 50 ℃ of stirrings of constant temperature water bath 4h, obtains the faint yellow TiO of homogeneous transparent
2Wet colloidal sol leaves standstill after 15 hours subsequent use;
(4) preparation TiO
2Xerogel: with TiO
2Wet colloidal sol in 70 ℃ of dry 48h, obtains TiO in vacuum drying oven
2Xerogel;
(5) preparation TiO
2Powder: with TiO
2After xerogel ground, in 600 ℃ of calcining 2h, temperature rise rate was 10 ℃/min under oxidizing atmosphere and normal pressure, to the TiO that obtains after above-mentioned calcining and activating and the cooling
2Powder grinds, and promptly obtains to have the TiO of photocatalytic activity
2Powder.
Wherein said stirring velocity is 300r/min, and rate of addition is 1ml/min in the step (1), and rate of addition is 0.4ml/min in the step (3).
The TiO of preparation
2Each crystal content of powder is: anatase octahedrite 92wt%, rutile 8wt%
With the mercury lamp is light source, and radiation 10min, its degradation rate are 91.2%; With the Metal-halogen lamp is light source, and radiation 10min, its degradation rate are 12.3%.
Claims (6)
1. TiO with visible light catalysis activity
2Powder is characterized in that the crystalline phase composition, is by weight percentage: Detitanium-ore-type TiO
2: 90-100wt%, rutile TiO
2: 0-10wt%.
2. a kind of TiO according to claim 1 with visible light catalysis activity
2The preparation method of powder is characterized in that carrying out according to following steps:
(1) preparation precursor liquid A: the 5-25ml tetra-n-butyl titanate is added drop-wise in the 10-35ml absolute ethyl alcohol while stirring, splashes into the 1-10ml Glacial acetic acid min. 99.5 again, through the stirring of 20-50min, the yellow solution that obtains homogeneous transparent is precursor liquid A;
(2) preparation dropping liquid B: with 5-20ml redistilled water and 5-15ml absolute ethyl alcohol wiring solution-forming, add hydrochloride adjusted solution pH value, stir 10-30min, obtain the dropping liquid B of pH value for 1-5;
(3) preparation TiO
2Wet colloidal sol: dropping liquid B is added drop-wise among the precursor liquid A, in water-bath, after 50-70 ℃ of constant temperature stirs 2h-4h, obtains the faint yellow TiO of homogeneous transparent
2Wet colloidal sol leaves standstill after 15 hours subsequent use;
(4) preparation TiO
2Xerogel: with the TiO that obtains
2Wet colloidal sol in 50-80 ℃ of dry 24-72h, obtains TiO in vacuum drying oven
2Xerogel;
(5) preparation TiO
2Powder: with TiO
2After xerogel ground, in 400-600 ℃ of calcining 2-5h, temperature rise rate was 5-10 ℃/min under oxidizing atmosphere and normal pressure, to calcining and be cooled to the TiO that obtains after the room temperature
2Powder grinds, and promptly obtains to have the nano-TiO of photocatalytic activity
2Powder.
3. a kind of TiO according to claim 2 with visible light catalysis activity
2The preparation method of powder is characterized in that the stirring velocity described in step (1), (2) and (3) is 200-300r/min.
4. a kind of TiO according to claim 2 with visible light catalysis activity
2The preparation method of powder is characterized in that the rate of addition described in the step (1) for being (0.7-1) ml/min, and the rate of addition in the step (3) is (0.1-0.4) ml/min.
5. a kind of TiO according to claim 2 with visible light catalysis activity
2The preparation method of powder is characterized in that the concentration of hydrochloric acid described in the step (2) is (0.1-0.12) mol/l.
6. a kind of TiO according to claim 2 with visible light catalysis activity
2The preparation method of powder is characterized in that the nano-TiO for preparing
2The crystalline phase of powder is formed, and is by weight percentage: Detitanium-ore-type TiO
2: 90-100wt%, rutile TiO
2: 0-10wt%.
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| CN103991903A (en) * | 2014-06-04 | 2014-08-20 | 江苏大学 | Method for preparing mixed-phase titanium dioxide nanosheet photocatalyst |
| CN104255797A (en) * | 2014-08-25 | 2015-01-07 | 中国海洋大学 | A silver/titanium oxide nanotube antifouling agent interfacially modified by polydopamine and a preparing method thereof |
| CN104528821A (en) * | 2014-12-29 | 2015-04-22 | 柳州邦诚科技有限公司 | Method for preparing nanometer titania |
| CN104607164A (en) * | 2015-01-16 | 2015-05-13 | 吉林化工学院 | Novel preparation method of photocatalytic material |
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| CN106882840A (en) * | 2017-01-25 | 2017-06-23 | 中国矿业大学 | It is a kind of to have visible light-responded TiO2Hierarchy and preparation method thereof |
| CN108043389A (en) * | 2017-12-19 | 2018-05-18 | 哈尔滨工业大学 | A kind of doped transition metal ions are modified TiO2The method of visible light catalysis activity |
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| CN104528821A (en) * | 2014-12-29 | 2015-04-22 | 柳州邦诚科技有限公司 | Method for preparing nanometer titania |
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| CN106882840B (en) * | 2017-01-25 | 2019-03-22 | 中国矿业大学 | It is a kind of to have visible light-responded TiO2Hierarchical structure and preparation method thereof |
| CN108043389A (en) * | 2017-12-19 | 2018-05-18 | 哈尔滨工业大学 | A kind of doped transition metal ions are modified TiO2The method of visible light catalysis activity |
| CN110314647A (en) * | 2019-06-28 | 2019-10-11 | 咸阳职业技术学院 | A kind of complex coal adsorbing material and preparation method thereof |
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