CN101357329A - Preparation method of vanadium-doped nano titanic oxide catalyst - Google Patents
Preparation method of vanadium-doped nano titanic oxide catalyst Download PDFInfo
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- CN101357329A CN101357329A CNA2008100416647A CN200810041664A CN101357329A CN 101357329 A CN101357329 A CN 101357329A CN A2008100416647 A CNA2008100416647 A CN A2008100416647A CN 200810041664 A CN200810041664 A CN 200810041664A CN 101357329 A CN101357329 A CN 101357329A
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Abstract
The invention relates a preparation method of a vanadium-doped nano titanium dioxide catalyst, which pertains to the field of nano-photocatalysis material. The preparation method comprises the steps as follows: (1) a precursor of titanium is dissolved in absolute ethyl alcohol, added with glacial acetic acid to inhibit the hydrolysis of the precursor, and evenly stirred to obtain solution A; (2) vanadate is weighed according to 0.1-1% of V/Ti mass ratio, put into deionized water or nitric acid or ammonia water for thorough dissolution and evenly stirred to obtain solution B; (3) the solution B is slowly dropped into the solution A which is stirred vigorously by a constant pressure funnel and stirred into a sol; then the sol obtained is transferred to a high pressure reaction kettle, and is kept in an oven for carrying out hydrothermal reaction; (4) the solution obtained is dried and ground to obtain a powdery product. In the photocatalyst produced by the preparation method of the invention, the average grain size is 10-20nm. By doping the vanadium, the forbidden band width of the nano titanium dioxide is reduced to the extent (400-800nm) which can make use of visible light, so that the visible-light catalytic activity is obviously improved.
Description
Technical field
The present invention relates to a kind of preparation method of nano-photocatalyst material technical field, specifically is a kind of preparation method of vanadium-doped nano titanic oxide catalyst.
Background technology
Photochemical catalytic oxidation at home and abroad is widely studied in recent years as a kind of potential and ideal environment improvement technology.In the research of semiconductor nano photochemical catalyst, TiO
2Because of advantage such as have good energy gap, oxidability is strong, catalytic activity is high, nontoxic, biological, chemistry, photochemical stability are good, be in the core status of photocatalysis in studying always.But TiO
2The band-gap energy broad can only use ultraviolet excitation, and the ultraviolet light in the sunshine accounts for 3%, is difficult to effectively utilize sunshine; Another problem is that the right recombination probability of semiconductor photoproduction electrons/is higher.The main path that addresses the above problem is to TiO
2Catalyst carries out modification, promptly changes particle structure and surface nature, thereby enlarges the photoresponse scope, and it is compound to improve quantum efficiency to suppress carrier, improves the stability and the photocatalytic activity of catalysis material.The doping of metal ion is a kind of effective modification technology.TiO
2In mix some metal (ion) modification after, impurity energy level has been introduced in the participation of metal, and may respond to some extent under excited by visible light, drives light-catalyzed reaction and carries out.Secondly, an amount of being doped with is beneficial to light induced electron and separates effectively with the hole, suppressed compound, thereby carrier lifetime is prolonged, and improved photo-quantum efficiency and photocatalytic activity.The 3rd, the doping of metal ion can reduce particle size, increases specific area, increases the stability of anatase etc.Therefore, to have than bigger serface, Detitanium-ore-type structure, the nano-powder that mixes metal ion be to improve TiO in preparation
2One of effective way of photocatalytic activity.
Sol-gel process is TiO
2The common method of mixing, foreign ion can be evenly dispersed in the reaction system in sol-gel process, and the solid solution that comprises metal impurities ion and titanium dioxide like this forms easily, and perhaps metal ion mixes TiO easily
2Lattice in.And the heat endurance that the material by Hydrothermal Preparation has perfect crystal structure, less crystallite dimension to become reconciled.In view of sol-gel process and hydro-thermal method advantage separately, the present invention carries out hydrothermal treatment consists again with sol-gel process and hydro-thermal method combination behind the collosol and gel, reach the purpose of crystallization.And characterize by X-ray diffraction (XRD), UV, visible light diffuse reflectance spectra (UV-Vis DRS) sample to preparation.By the liquid phase photocatalytic degradation of dyestuff Acid Orange II being verified the raising of the visible light catalysis activity of vanadium doped samples.
Find through literature search prior art, " mixing the visible light catalytic performance study of vanadium titanium dioxide " that Guan Jing etc. deliver on " application chemical industry " (second phase 117-119 page or leaf in 2006) proposes to prepare visible-light response type with sol-gel process and mixes vanadium TiO in this article
2The method of photochemical catalyst, but it is to be the TiO that light source carries out with fluorescent lamp (simulated solar irradiation)
2Catalytically active assessment, and calcining heat is too high about 700 ℃.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of preparation method of vanadium-doped nano titanic oxide catalyst is provided, the present invention adopts back hydrothermal treatment consists technology, can significantly reduce calcining heat.In addition, adopting light source is iodine-tungsten lamp irradiation the carrying out photocatalysis test (with the light of filter plate elimination wavelength less than 450nm) of 500W, reacts completely and carries out under visible light, has got rid of the influence of ultraviolet light.The average grain size of the composite photo-catalyst that the present invention prepares is at 10-20nm, and powder is dispersity substantially, and the doping of v element has suppressed nano-TiO
2The transformation of crystal formation; Material still is pure anatase type structure when 500 ℃ of calcinings after tested.
The present invention is achieved through the following technical solutions, and the present invention includes following steps:
The first step is dissolved in the precursor of titanium in the absolute ethyl alcohol, adds glacial acetic acid and suppresses its hydrolysis, evenly stirs into A liquid;
Second step took by weighing vanadate with the V/Ti mass ratio of 0.1%-1%, placed deionized water or nitric acid or ammoniacal liquor that it is dissolved fully, evenly stirred and formed B liquid;
In the 3rd step, B liquid slowly splashes into to stir in the A liquid of vigorous stirring through constant pressure funnel and forms colloidal sol; Change gained colloidal sol over to autoclave again, and in baking oven, place the generation hydro-thermal reaction;
In the 4th step,, obtain the powder product with gained solution drying, grinding.
The precursor of described titanium comprises the inorganic salts of titanium alkoxide and titanium, and titanium alcohol salt comprises a kind of in butyl titanate, the tetraethyl titanate etc.; The inorganic salts of titanium are a kind of in titanium chloride, the titanium sulfate etc.
Described vanadate is a kind of in ammonium metavanadate, sodium metavanadate, the potassium metavanadate etc.
Described nitric acid is red fuming nitric acid (RFNA), and its pH is between 1.5-2.0.
Slightly solubles such as described ammonium metavanadate or be insoluble in the material of water, available ammoniacal liquor, 80 ℃-100 ℃ hot water dissolving.
Institute is set forth in places in the baking oven, and be 8h-12h its standing time.
Described hydro-thermal reaction, its temperature are 120 ℃-180 ℃, and made vanadium-doped nano titanic oxide is Detitanium-ore-type, are regular Detitanium-ore-type crystal structure after 250 ℃ of-300 ℃ of calcinings.
Described grinding also can be ground behind calcining 3h.
Among the present invention, following method is adopted in prepared material photocatalytic properties test:
Target degradation product: 20mg/l Acid Orange II solution;
The visible light catalysis activity test of sample: adopting light source is iodine-tungsten lamp irradiation the carrying out photocatalysis test (with the light of filter plate elimination wavelength less than 450nm) of 500W, and lamp is 10cm to the distance at quartz test tube center.Iodine-tungsten lamp cools off with the recirculated water in the quartzy chuck, and reaction system is lowered the temperature with the 15W fan, and system temperature remains essentially in about 40 ℃.
Under the lucifuge condition, stir 1h and guarantee that reactant reaches balance in the absorption of sample surfaces.The illumination 5h that turns on light then takes a sample with syringe every 1h, and the amount of each solution of getting is about 5ml, and centrifuge (12,000 rev/mins) went supernatant liquor to place cuvette in centrifugal 5-8 minute, surveyed its absorbance and tried to achieve dye decolored rate.Each light degradation experiment repeats 3 times, averages, and error is no more than 5%.Adopt the light absorption value (A) of ultraviolet-visible spectrophotometer (484nm) working sample under maximum absorption wavelength.Between the absorbance A of the concentration range inner acidic of the 0-50mg/L orange II aqueous solution and concentration, meet Lambert-Beer's law, so formula calculates the degradation rate of dyestuff below available.
In the formula, C
0Be the initial concentration after the pre-absorption of dyestuff Acid Orange II; C is each reaction density when getting Acid Orange II; A
0For adsorb the light absorption value under the initial concentration of back in advance at Acid Orange II under the 484nm wavelength; A is the each down light absorption value of getting under the Acid Orange II reaction density of 484nm wavelength.
The present invention adopts collosol and gel-hydro-thermal synthetic technology to prepare the vanadium-doped nano titanic oxide material, improve the method for its visible light catalysis activity, this method is incorporated into v element in the nano titanium oxide lattice, and fractional load being arranged on its surface, the average grain size of gained photochemical catalyst is at 10-20nm.Mix by vanadium, the energy gap of nano titanium oxide can be reduced to the degree (400-800nm) that can utilize visible-range, visible light catalysis activity obviously improves.
Description of drawings
Fig. 1 is the titania-doped ultraviolet-visible absorption spectroscopy schematic diagram of vanadium.
Fig. 2 is the XRD signal collection of illustrative plates of the titania-doped 300 ℃ of calcinings of vanadium.
The specific embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
For the vanadium doping ferrous oxide that confirms high catalytic activity under the visible light absorbent properties to light, (UV-vis) is measured for uv-visible absorption spectra.Measuring instrument is VARIAN Cary 500 UV-visspectrophotometer.As shown in Figure 1, this ultraviolet-visible absorption spectroscopy measuring instrument is VARIAN Cary500UV-vis spectrophotometer.In whole visible wavelength 360-700nm, the titania-doped absorbance of vanadium is higher than pure nano titanium oxide, and its spectral absorption sideband extends to about 550nm from about the 385nm of pure nano titanium oxide.Absorb sideband obvious red shift has taken place, i.e. the spectral response range of the titanium oxide nanoparticles that explanation is mixed is expanded to visible region.
As shown in Figure 2, the XRD figure spectrometry instrument of this calcining is a D/max2200VPC polycrystalline X-ray diffractometer.Simultaneously as can be known to the titania-doped XRD figure analysis of spectrum of Fig. 2 part vanadium, 300 ℃ down calcining have only anatase phase to form, can estimate that according to the Scherrer formula its particle diameter is about 10～14nm.
Embodiment one:
Under the room temperature 10ml butyl titanate is added in the 10ml absolute ethyl alcohol, add glacial acetic acid and suppress its hydrolysis, be stirred into solution A, be placed in the separatory funnel.
Take by weighing ammonium metavanadate by 0.1% (vanadium titanium mass ratio) doping ratio, add appropriate amount of deionized water, red fuming nitric acid (RFNA) dissolving (pH is 1.5-2) claims solution B.
Under magnetic agitation, slowly be added drop-wise in the solution A solution B, obtain the colloidal sol of homogeneous transparent, then with its taking-up, put into the autoclave that liner is a polytetrafluoroethylene (PTFE), in 120 ℃ of heating 8h, the titania powder that obtains mixing, take out, with distilled water washing, drying,, grind and promptly obtain required nano particle after the centrifugation 300 ℃ of calcinings.Products therefrom is by above-mentioned photocatalytic activity method of testing, and recording its percent of decolourization to Acid Orange II is 80%, has very strong visible light catalysis activity.
Embodiment two:
Under the room temperature 10ml tetraethyl titanate is added in the 10ml absolute ethyl alcohol, add glacial acetic acid and suppress its hydrolysis, be stirred into solution A, be placed in the separatory funnel.
Take by weighing sodium metavanadate by 0.1% (vanadium titanium mass ratio) doping ratio, add appropriate amount of deionized water and make it dissolve the formation solution B fully.
Under magnetic agitation, slowly be added drop-wise in the solution A solution B, obtain the colloidal sol of homogeneous transparent, then with its taking-up, put into the autoclave that liner is a polytetrafluoroethylene (PTFE), in 150 ℃ of heating 8h, the titania powder that obtains mixing, take out, with distilled water washing, drying,, grind and promptly obtain required nano particle after the centrifugation 250 ℃ of calcinings.Products therefrom is through the photocatalytic activity experiment test, and the percent of decolourization of Acid Orange II is 85%.
Embodiment three:
With stirring in the 10ml butyl titanate adding 10ml absolute ethyl alcohol, be called for short solution A under the room temperature, be placed in the separatory funnel.
Take by weighing ammonium metavanadate by 0.2% (vanadium titanium mass ratio) doping ratio, add appropriate amount of deionized water and concentrated ammonia liquor to ammonium metavanadate and dissolve fully, claim solution B.
Under magnetic agitation, slowly be added drop-wise in the solution A solution B, obtain the colloidal sol of homogeneous transparent, then with its taking-up, put into the autoclave that liner is a polytetrafluoroethylene (PTFE), in 150 ℃ of heating 12h, the titania powder that obtains mixing, take out, with distilled water washing, drying,, grind and promptly obtain required nano particle after the centrifugation 250 ℃ of calcinings.Products therefrom is through the photocatalytic activity experiment test, and the percent of decolourization of Acid Orange II is 80%.
Embodiment four:
Under the room temperature 10ml titanium tetrachloride is added in the 15ml absolute ethyl alcohol, in ice water bath environment, stir, be called for short solution A, be placed in the separatory funnel.
Take by weighing ammonium metavanadate respectively by 0.5% (vanadium titanium mass ratio) doping ratio, add appropriate amount of deionized water and concentrated ammonia liquor to ammonium metavanadate and dissolve fully, claim solution B.
Under magnetic agitation, slowly be added drop-wise in the solution A solution B, obtain the colloidal sol of homogeneous transparent, then with its taking-up, put into the autoclave that liner is a polytetrafluoroethylene (PTFE), in 180 ℃ of heating 12h, the titania powder that obtains mixing takes out, with distilled water washing, dry back fine gtinding, promptly obtain required nano particle after the centrifugation.Because of products therefrom without calcining, it has showed stronger absorption property in photocatalytic process, the percent of decolourization of photocatalytic activity test Acid Orange II reaches more than 95%.
Claims (10)
1, a kind of preparation method of vanadium-doped nano titanic oxide catalyst is characterized in that comprising the steps:
The first step is dissolved in the precursor of titanium in the absolute ethyl alcohol, adds glacial acetic acid and suppresses its hydrolysis, evenly stirs into A liquid;
Second step took by weighing vanadate with the V/Ti mass ratio of 0.1%-1%, placed deionized water or nitric acid or ammoniacal liquor that it is dissolved fully, evenly stirred and formed B liquid;
In the 3rd step, B liquid slowly splashes into to stir in the A liquid of vigorous stirring through constant pressure funnel and forms colloidal sol; Change gained colloidal sol over to autoclave again, and in baking oven, place the generation hydro-thermal reaction;
In the 4th step,, obtain the powder product with gained solution drying, grinding.
2, the preparation method of vanadium-doped nano titanic oxide catalyst according to claim 1 is characterized in that: the precursor of described titanium is a kind of in the inorganic salts of titanium alkoxide and titanium.
3, the preparation method of vanadium-doped nano titanic oxide catalyst according to claim 2 is characterized in that: titanium alcohol salt comprises a kind of in butyl titanate, the tetraethyl titanate.
4, the preparation method of vanadium-doped nano titanic oxide catalyst according to claim 2 is characterized in that: the inorganic salts of titanium are a kind of in titanium chloride, the titanium sulfate.
5, the preparation method of vanadium-doped nano titanic oxide catalyst according to claim 1 is characterized in that: described vanadate is a kind of in ammonium metavanadate, sodium metavanadate, the potassium metavanadate.
6, the preparation method of vanadium-doped nano titanic oxide catalyst according to claim 1 is characterized in that: described nitric acid is red fuming nitric acid (RFNA), and its pH is between 1.5-2.0.
7, the preparation method of vanadium-doped nano titanic oxide catalyst according to claim 1 is characterized in that: described ammonium metavanadate is with ammoniacal liquor, 80 ℃-100 ℃ hot water dissolving.
8, the preparation method of vanadium-doped nano titanic oxide catalyst according to claim 1 is characterized in that: institute is set forth in places in the baking oven, and be 8h-12h its standing time.
9, the preparation method of vanadium-doped nano titanic oxide catalyst according to claim 1, it is characterized in that: described hydro-thermal reaction, its temperature is 120 ℃-180 ℃, and made vanadium-doped nano titanic oxide is Detitanium-ore-type, is regular Detitanium-ore-type crystal structure after 250 ℃ of-300 ℃ of calcinings.
10, the preparation method of vanadium-doped nano titanic oxide catalyst according to claim 1 is characterized in that: described grinding or carry out behind the 3h in calcining.
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