CN102765758B - Sol-gel-hydrothermal method for preparing bismuth tungstate and indium-doped bismuth tungstate - Google Patents
Sol-gel-hydrothermal method for preparing bismuth tungstate and indium-doped bismuth tungstate Download PDFInfo
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Abstract
The invention discloses a sol-gel-hydrothermal method for preparing bismuth tungstate and indium-doped bismuth tungstate. The technical scheme point of the invention is to respectively disclose a sol-gel-hydrothermal method for preparing a bismuth tungstate catalyst and a sol-gel-hydrothermal method for preparing an indium-doped bismuth tungstate catalyst. The preparation method disclosed by the invention has the advantages of simple operation and low cost; and the prepared bismuth tungstate catalyst and the indium-doped bismuth tungstate catalyst have excellent photocatalysis performance.
Description
Technical field
The present invention relates to a kind of bismuth tungstate (Bi
2wO
6) and the preparation method of indium doping bismuth tungstate, belong to inorganic functional material field, particularly a kind of sol-gel-hydrothermal is prepared the method for bismuth tungstate and indium doping bismuth tungstate.
Background technology
Environmental pollution is the significant challenge that current mankind faces, and utilizing photocatalysis technology to administer environmental problem is one of current most active research field, finds the top priority that high efficiency photocatalyst is this field.Early stage research mainly concentrates on TiO
2, it has, and catalytic activity is high, good stability, low price, the premium properties such as nontoxic, thereby enjoys favor.But TiO
2energy gap is 3.2eV, only under wavelength is less than the ultraviolet ray of 387nm, just can excite its catalytic activity.In arriving the sun power on ground, the energy of this wave band is less than 5% still, and the ratio of visible light part accounts for 45% left and right of sun power.Therefore, the visible light catalyst of the efficient response of design becomes photochemical catalysis science and pollutes and control one of great research topic facing.
Bismuth tungstate (Bi
2wO
6) photocatalyst is with its unique electronic structure, good visible absorption ability and higher organic matter degradation ability, is considered to a kind of potential good visible light catalytic material.The preparation method of bismuth tungstate mainly concentrates on coprecipitation method, sol-gel method and hydrothermal method etc. at present.But coprecipitation method and sol-gel method all need high-temperature calcination just can obtain crystallinity bismuth tungstate in preparation process, and pyroprocess can directly cause crystal grain reunite and size distribution inhomogeneous, thereby reduce the photocatalysis performance of bismuth tungstate; Hydrothermal method is prepared bismuth tungstate and has been saved high-temperature calcination link, and products obtained therefrom has complete in crystal formation and purity advantages of higher, but uses this method to be unfavorable for the composite mixed of multiple element, and bismuth tungstate is carried out to doping treatment, is to improve the most important method of its photocatalytic activity.Therefore, study that a kind of to prepare the bismuth tungstate photocatalyst novel method with high catalytic activity particularly necessary.Bismuth tungstate being carried out to doping treatment and can effectively reduce the compound of light induced electron-hole, is the important method that improves its photocatalytic activity, therefore, studies and a kind ofly prepares that to have the doping bismuth tungstate photocatalyst of high catalytic activity also particularly important.
Summary of the invention
The technical problem that the present invention solves has been to provide a kind of method that sol-gel-hydrothermal is prepared bismuth tungstate, adopt the method in sol-gel process, to adulterate, then carry out hydro-thermal reaction, can overcome and existingly prepare that crystal grain in bismuth tungstate method is easily reunited, the shortcoming of difficult doping, prepare that particle diameter is little, reunion degree is low, complete in crystal formation, the easy nanometer bismuth tungstate photocatalyst of doping.
Another technical problem that the present invention solves has been to provide a kind of method that sol-gel-hydrothermal is prepared indium doping bismuth tungstate, the method is in sol-gel process, to be doped into phosphide element, and then carries out hydro-thermal reaction and the indium doping bismuth tungstate photocatalyst Bi that forms
2-
x in
x wO
6(0.01≤
x≤ 0.1).
Technical scheme of the present invention is: a kind of sol-gel-hydrothermal is prepared the method for bismuth tungstate, it is characterized in that comprising the following steps: (1), with ammonium tungstate (H
40n
10o
41w
12), Bismuth trinitrate (Bi (NO
3)
3), EDTA and deionized water be raw material, respectively ammonium tungstate and Bismuth trinitrate and deionized water are made into the aqueous solution, then under the condition stirring, add EDTA solution to form clear solution respectively in ammonium tungstate solution and bismuth nitrate solution, wherein in ammonium tungstate solution, the add-on of EDTA is n(EDTA): n(H
40n
10o
41w
12)=18:1, in bismuth nitrate solution, the add-on of EDTA is n(EDTA): n(Bi (NO
3)
3)=1.5:1; (2), by the clear solution of step (1) gained n(H in molar ratio
40n
10o
41w
12): n (Bi (NO
3)
3the ratio of)=1:24 mixes, and then the transparent mixed solution of gained is kept in the water-bath of 60 ~ 80 ℃ 12 ~ 24 hours obtaining to wet gel, and wet gel is dried to obtain xerogel through 110 ℃; (3), the xerogel of step (2) gained is moved in hydrothermal reaction kettle, with acid or alkali, regulating the pH value of reaction soln is 2 ~ 11, then at 180 ~ 240 ℃, keep after 6 ~ 36 hours, through coldly going, filter, wash, after dry, obtain having the bismuth tungstate photocatalyst of high catalytic activity.Sol-gel-hydrothermal of the present invention is prepared the method for bismuth tungstate, it is characterized in that: in described step (1), the volumetric molar concentration of ammonium tungstate solution and bismuth nitrate solution is 0.001 ~ 0.5mol/L.Sol-gel-hydrothermal of the present invention is prepared the method for bismuth tungstate, it is characterized in that: in described step (1), the volumetric molar concentration of EDTA solution is 0.01 ~ 0.5mol/L.Sol-gel-hydrothermal of the present invention is prepared the method for bismuth tungstate, it is characterized in that: the acid in described step (3) can be nitric acid, and alkali can be ammoniacal liquor.
A kind of sol-gel-hydrothermal is prepared the method for indium doping bismuth tungstate, it is characterized in that: in the sol-gel process in the preparation method of above-mentioned bismuth tungstate, add indium nitrate to form indium doping bismuth tungstate photocatalyst, its concrete steps are: (1), with ammonium tungstate (H
40n
10o
41w
12), Bismuth trinitrate (Bi (NO
3)
3), indium nitrate (In (NO
3)
3), EDTA and deionized water be raw material, ammonium tungstate, Bismuth trinitrate and indium nitrate and deionized water are made into the aqueous solution, then under the condition stirring, add EDTA solution to form clear solution respectively in ammonium tungstate solution, bismuth nitrate solution and indium nitrate solution, wherein in ammonium tungstate solution, the add-on of EDTA is n(EDTA): n(H
40n
10o
41w
12)=18:1, in bismuth nitrate solution, the add-on of EDTA is n(EDTA): n(Bi (NO
3)
3)=1.5:1, in indium nitrate solution, the add-on of EDTA is n(EDTA): n(In (NO
3)
3)=1.5:1; (2), according to Bi
2-
x in
x wO
6(0.01≤
x≤ 0.1) stoichiometric ratio mixes three kinds of clear solutions of step (1) gained, then the transparent mixed solution of gained is kept in the water-bath of 80 ℃ 24 hours obtaining to wet gel, and wet gel is dried to obtain xerogel through 110 ℃; (3), the xerogel of step (2) gained is moved in hydrothermal reaction kettle, with acid or alkali, regulating the pH value of reaction soln is 2 ~ 11, then at 180 ~ 240 ℃, keeps after 6 ~ 36 hours, through the cold Bi that obtains having high catalytic activity after going, filter, wash, being dried
2-
x in
x wO
6(0.01≤
x≤ 0.1) photocatalyst.Sol-gel-hydrothermal of the present invention is prepared the method for indium doping bismuth tungstate, it is characterized in that: in described step (1), the volumetric molar concentration of ammonium tungstate solution, bismuth nitrate solution and indium nitrate solution is 0.001 ~ 0.5mol/L.Sol-gel-hydrothermal of the present invention is prepared the method for indium doping bismuth tungstate, it is characterized in that: the volumetric molar concentration of described step (1) EDTA solution is 0.01 ~ 0.5mol/L.Sol-gel-hydrothermal of the present invention is prepared the method for bismuth tungstate, it is characterized in that: the acid in described step (3) can be nitric acid, and alkali can be ammoniacal liquor.
Gained bismuth tungstate photocatalyst crystal property of the present invention is good, and pattern is that pleat is spherical, has larger specific surface area and good photocatalytic activity.Method of the present invention has overcome existingly prepares that crystal grain in bismuth tungstate method is easily reunited, the shortcoming of difficult doping, has prepared that particle diameter is little, reunion degree is low, complete in crystal formation, the nanometer bismuth tungstate photocatalyst of easily doping and the nanometer bismuth tungstate photocatalyst of indium doping.
Accompanying drawing explanation
Fig. 1 is the bismuth tungstate (Bi of the embodiment of the present invention 1 preparation
2wO
6) X-ray diffractogram.
Embodiment
Further describe with the following Examples the present invention.Be noted that the present invention is not limited to following each embodiment.
Embodiment 1
(1), compound concentration is each 10mL of ammonium tungstate solution that 0.024mol/L bismuth nitrate solution and concentration are 0.001mol/L, under the condition stirring, the EDTA solution that 3.6mL and 1.8mL concentration is to 0.1mol/L joins respectively in bismuth nitrate solution and ammonium tungstate solution;
(2), in the water-bath of 60 ℃, keep 24 hours obtaining wet gel after above-mentioned two kinds of clear solutions are mixed, wet gel is through 110 ℃ of dry xerogel that to obtain;
(3), xerogel is moved in hydrothermal reaction kettle, add 50ml deionized water and with nitric acid, regulate the pH=2.0 of reaction soln, then at 220 ℃, keep, after 12 hours, naturally cooling to room temperature.To obtain product centrifugation, use deionized water wash 3 times, after 60 ℃ of vacuum-drying, obtain having the bismuth tungstate photocatalyst of high catalytic activity, from X ray diffracting spectrum, can find out that it is consistent with the crystalline structure of bismuth tungstate.
Embodiment 2
(1), compound concentration is each 10mL of ammonium tungstate solution that 0.24mol/L bismuth nitrate solution and concentration are 0.01mol/L, under the condition stirring, the EDTA solution that respectively 7.2mL and 3.6mL concentration is to 0.5mol/L joins in bismuth nitrate solution and ammonium tungstate solution;
(2), in the water-bath of 80 ℃, keep 24 hours obtaining wet gel after above-mentioned two kinds of clear solutions are mixed, wet gel is through 110 ℃ of dry xerogel that to obtain;
(3), xerogel is moved in hydrothermal reaction kettle, add 50ml deionized water and with ammoniacal liquor, regulate the pH=11.0 of reaction soln, then at 240 ℃, keep, after 6 hours, naturally cooling to room temperature.To obtain product centrifugation, use deionized water wash 3 times, after 60 ℃ of vacuum-drying, obtain having the bismuth tungstate photocatalyst of high catalytic activity.
Embodiment 3
(1), compound concentration is each 10mL of ammonium tungstate solution that 0.12mol/L bismuth nitrate solution and concentration are 0.005mol/L, under the condition stirring, the EDTA solution that respectively 3.6mL and 1.8mL concentration is to 0.5mol/L joins in bismuth nitrate solution and ammonium tungstate solution;
(2), in the water-bath of 60 ℃, keep 12 hours obtaining wet gel after above-mentioned two kinds of clear solutions are mixed, wet gel is through 110 ℃ of dry xerogel that to obtain;
(3), xerogel is moved in hydrothermal reaction kettle, add 50ml deionized water and with nitric acid, regulate the pH=2.0 of reaction soln, then at 180 ℃, keep, after 36 hours, naturally cooling to room temperature.To obtain product centrifugation, use deionized water wash 3 times, after 60 ℃ of vacuum-drying, obtain having the bismuth tungstate photocatalyst of high catalytic activity.
Embodiment 4
(1), compound concentration is 0.24mol/L bismuth nitrate solution 99.5mL, compound concentration is 0.024mol/L indium nitrate solution 5mL, compound concentration is the ammonium tungstate solution 100mL of 0.01mol/L, under the condition stirring, the EDTA solution that respectively 71.64mL, 0.36mL and 36mL concentration is to 0.5mol/L joins in bismuth nitrate solution, indium nitrate solution and ammonium tungstate solution;
(2), in the water-bath of 80 ℃, keep 24 hours obtaining wet gel after above-mentioned clear solution is mixed, wet gel is through 110 ℃ of dry xerogel that to obtain;
(3), xerogel is moved in hydrothermal reaction kettle, add 100ml deionized water and with ammoniacal liquor, regulate the pH=11.0 of reaction soln, then at 240 ℃, keep, after 6 hours, naturally cooling to room temperature.To obtain product centrifugation, use deionized water wash 3 times, after 60 ℃ of vacuum-drying, obtain having the Bi of high catalytic activity
1.99in
0.01wO
6photocatalyst.
Embodiment 5
(1), compound concentration is 0.024mol/L bismuth nitrate solution 97.5mL, compound concentration is 0.012mol/L indium nitrate solution 5mL, compound concentration is the ammonium tungstate solution 100mL of 0.001mol/L, under the condition stirring, the EDTA solution that 35.1mL, 0.9mL and 18mL concentration is to 0.1mol/L joins respectively in Bismuth trinitrate, indium nitrate and ammonium tungstate solution;
(2), in the water-bath of 80 ℃, keep 24 hours obtaining wet gel after above-mentioned clear solution is mixed, wet gel is through 110 ℃ of dry xerogel that to obtain;
(3), xerogel is moved in hydrothermal reaction kettle, add 100ml deionized water and with nitric acid, regulate the pH=3.0 of reaction soln, then at 220 ℃, keep, after 12 hours, naturally cooling to room temperature.To obtain product centrifugation, use deionized water wash 3 times, after 60 ℃ of vacuum-drying, obtain having the Bi of high catalytic activity
1.95in
0.05wO
6photocatalyst.
Embodiment 6
(1), compound concentration is 0.12mol/L bismuth nitrate solution 95mL, compound concentration is 0.012mol/L indium nitrate solution 5mL, compound concentration is the ammonium tungstate solution 100mL of 0.005mol/L, under the condition stirring, the EDTA solution that respectively 34.2mL, 1.8mL and 18mL concentration is to 0.5mol/L joins in Bismuth trinitrate and ammonium tungstate solution;
(2), in the water-bath of 80 ℃, keep 24 hours obtaining wet gel after above-mentioned clear solution is mixed, wet gel is through 110 ℃ of dry xerogel that to obtain;
(3), xerogel is moved in hydrothermal reaction kettle, add 100ml deionized water and with nitric acid, regulate the pH=2.0 of reaction soln, then at 180 ℃, keep, after 36 hours, naturally cooling to room temperature.To obtain product centrifugation, use deionized water wash 3 times, after 60 ℃ of vacuum-drying, obtain having the Bi of high catalytic activity
1.9in
0.1wO
6photocatalyst.
Above embodiment has described ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; do not departing under the scope of the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (8)
1. sol-gel-hydrothermal is prepared a method for bismuth tungstate, it is characterized in that comprising the following steps: (1), with ammonium tungstate (H
40n
10o
41w
12), Bismuth trinitrate (Bi (NO
3)
3), EDTA and deionized water be raw material, respectively ammonium tungstate and Bismuth trinitrate and deionized water are made into the aqueous solution, then under the condition stirring, add EDTA solution to form clear solution respectively in ammonium tungstate solution and bismuth nitrate solution, wherein in ammonium tungstate solution, the add-on of EDTA solution is n(EDTA): n(H
40n
10o
41w
12)=18:1, in bismuth nitrate solution, the add-on of EDTA solution is n(EDTA): n(Bi (NO
3)
3)=1.5:1; (2), by the clear solution of step (1) gained n(H in molar ratio
40n
10o
41w
12): n (Bi (NO
3)
3the ratio of)=1:24 mixes, and then the transparent mixed solution of gained is kept in the water-bath of 60-80 ℃ 12-24 hour obtaining to wet gel, and wet gel is dried to obtain xerogel through 110 ℃; (3), the xerogel of step (2) gained is moved in hydrothermal reaction kettle, add deionized water to form reaction soln, and be 2 ~ 11 by the pH value of acid or alkali adjusting reaction soln, then at 180-240 ℃, keep after 6-36 hour, through cooling, filter, washing, obtain having the bismuth tungstate photocatalyst of high catalytic activity after dry.
2. sol-gel-hydrothermal according to claim 1 is prepared the method for bismuth tungstate, it is characterized in that: in described step (1), the volumetric molar concentration of ammonium tungstate solution and bismuth nitrate solution is 0.001 ~ 0.5mol/L.
3. sol-gel-hydrothermal according to claim 1 is prepared the method for bismuth tungstate, it is characterized in that: the volumetric molar concentration of described step (1) EDTA solution is 0.01 ~ 0.5mol/L.
4. sol-gel-hydrothermal according to claim 1 is prepared the method for bismuth tungstate, it is characterized in that: the acid in described step (3) is nitric acid, and alkali is ammoniacal liquor.
5. a sol-gel-hydrothermal is prepared the method for indium doping bismuth tungstate, it is characterized in that: in the sol-gel process in the preparation method of bismuth tungstate described in claim 1, add indium nitrate to form indium doping bismuth tungstate photocatalyst, its concrete steps are: (1), with ammonium tungstate (H
40n
10o
41w
12), Bismuth trinitrate (Bi (NO
3)
3), indium nitrate (In (NO
3)
3), EDTA and deionized water be raw material, ammonium tungstate, Bismuth trinitrate and indium nitrate and deionized water are made into the aqueous solution, then under the condition stirring, add EDTA solution to form clear solution respectively in ammonium tungstate solution, bismuth nitrate solution and indium nitrate solution, wherein in ammonium tungstate solution, the add-on of EDTA is n(EDTA): n(H
40n
10o
41w
12)=18:1, in bismuth nitrate solution, the add-on of EDTA is n(EDTA): n(Bi (NO
3)
3)=1.5:1, in indium nitrate solution, the add-on of EDTA is n(EDTA): n(In (NO
3)
3)=1.5:1; (2), according to Bi
2-
x in
x wO
6stoichiometric ratio three kinds of clear solutions of step (1) gained are mixed, wherein 0.01≤
x≤ 0.1, then the transparent mixed solution of gained is kept in the water-bath of 80 ℃ 24 hours obtaining to wet gel, wet gel is dried to obtain xerogel through 110 ℃; (3), the xerogel of step (2) gained is moved in hydrothermal reaction kettle, add deionized water to form reaction soln, and be 2 ~ 11 by the pH value of acid or alkali adjusting reaction soln, then at 180-240 ℃, keep after 6-36 hour, through cooling, filter, washing, obtain having the Bi of high catalytic activity after dry
2-
x in
x wO
6photocatalyst, wherein 0.01≤
x≤ 0.1.
6. sol-gel-hydrothermal according to claim 5 is prepared the method for indium doping bismuth tungstate, it is characterized in that: in described step (1), the volumetric molar concentration of ammonium tungstate solution, bismuth nitrate solution and indium nitrate solution is 0.001 ~ 0.5mol/L.
7. sol-gel-hydrothermal according to claim 5 is prepared the method for indium doping bismuth tungstate, it is characterized in that: the volumetric molar concentration of described step (1) EDTA solution is 0.01 ~ 0.5mol/L.
8. sol-gel-hydrothermal according to claim 5 is prepared the method for indium doping bismuth tungstate, it is characterized in that: the acid in described step (3) is nitric acid, and alkali is ammoniacal liquor.
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| CN103623811B (en) * | 2013-09-12 | 2015-09-30 | 陕西科技大学 | The In-Bi that a kind of electron-hole recombination rate is low 2wO 6photochemical catalyst and preparation method thereof |
| CN103611559B (en) * | 2013-12-05 | 2015-06-03 | 河南师范大学 | Bi2WO6-SrTaO2N composite photocatalyst and preparation method thereof |
| CN103611528B (en) * | 2013-12-05 | 2015-06-03 | 河南师范大学 | Method for preparing bismuth tungstate catalyst by taking egg white as template |
| CN103818962B (en) * | 2013-12-30 | 2016-05-11 | 烟台佳隆纳米产业有限公司 | A kind of preparation method of caesium tungsten oxide superfine powder |
| CN105679546B (en) * | 2016-01-18 | 2017-12-19 | 黑龙江大学 | A kind of InWO4:Eu3+/TiO2Complex light anode and preparation method thereof |
| CN106732534B (en) * | 2016-11-29 | 2019-08-09 | 辽宁大学 | A kind of infrared ray excited bismuth tungstate photocatalyst and preparation method thereof |
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| CN102335602B (en) * | 2010-07-21 | 2013-07-17 | 中国科学院上海硅酸盐研究所 | Bismuth tungstate composite photocatalyst, preparation method thereof, and application thereof |
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