CN102765758A - 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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- CN102765758A CN102765758A CN2012102767184A CN201210276718A CN102765758A CN 102765758 A CN102765758 A CN 102765758A CN 2012102767184 A CN2012102767184 A CN 2012102767184A CN 201210276718 A CN201210276718 A CN 201210276718A CN 102765758 A CN102765758 A CN 102765758A
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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 the inorganic functional material field, the method for particularly a kind of sol-gel-Hydrothermal Preparation 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 present most active research field, seeks the top priority that high efficiency photocatalyst is this field.Early stage research mainly concentrates on TiO
2, it has catalytic activity height, good stability, low price, premium properties such as nontoxic, thereby enjoys favor.But TiO
2Energy gap is 3.2eV, only just can excite its catalytic activity at wavelength under less than the ultraviolet ray of 387nm.In the sun power that arrives ground, the energy of this wave band is less than 5% still, and the ratio of visible light part accounts for about 45% of sun power.Therefore, the visible light catalyst of design of High Efficiency response becomes the photochemical catalysis science and pollutes and control one of great research topic that is faced.
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 the good visible light catalytic material of a kind of potential.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 the crystallinity bismuth tungstate in the preparation process, and pyroprocess can directly cause crystal grain reunite and size distribution inhomogeneous, thereby reduce the photocatalysis performance of bismuth tungstate; The Hydrothermal Preparation bismuth tungstate has saved the 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, is to improve the most important method of its photocatalytic activity and bismuth tungstate is carried out doping treatment.Therefore, it is particularly necessary to study the bismuth tungstate photocatalyst novel method that a kind of preparation has a high catalytic activity.Bismuth tungstate being carried out doping treatment can effectively reduce the compound of light induced electron-hole, is the important method that improves its photocatalytic activity, and therefore, studying a kind of preparation, to have a doping bismuth tungstate photocatalyst of high catalytic activity also particularly important.
Summary of the invention
The technical problem that the present invention solves has provided the method for a kind of sol-gel-Hydrothermal Preparation bismuth tungstate; Adopt this method in sol-gel process, to mix; Carry out hydro-thermal reaction then; Can overcome that crystal grain is prone to reunite in the existing preparation bismuth tungstate method, difficult adulterated shortcoming, prepare that particle diameter is little, the reunion degree is low, complete in crystal formation, be prone to adulterated nanometer bismuth tungstate photocatalyst.
Another technical problem that the present invention solves has provided the method for a kind of sol-gel-Hydrothermal Preparation indium doping bismuth tungstate; This 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: the method for a kind of sol-gel-Hydrothermal Preparation bismuth tungstate is characterized in that may further comprise the 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; Under stirring condition, in ammonium tungstate solution and bismuth nitrate solution, add EDTA solution then respectively and form clear solution, wherein the add-on of EDTA is n (EDTA) in the ammonium tungstate solution: n (H
40N
10O
41W
12)=18:1, the add-on of EDTA is n (EDTA) in the bismuth nitrate solution: n (Bi (NO
3)
3)=1.5:1; (2), with the clear solution of step (1) gained n (H in molar ratio
40N
10O
41W
12): n (Bi (NO
3)
3The mixed of)=1:24 is even, and the transparent mixed solution with gained keeps getting in 12 ~ 24 hours wet gel in 60 ~ 80 ℃ water-bath then, and wet gel is through 110 ℃ of dry xerogel that get; (3), the xerogel with step (2) gained moves in the hydrothermal reaction kettle; Using the pH value of acid or alkali conditioned reaction solution is 2 ~ 11; Then 180 ~ 240 ℃ keep 6 ~ 36 hours after, through coldly removing, filter, wash, obtain having after the drying bismuth tungstate photocatalyst of high catalytic activity.The method of sol-gel of the present invention-Hydrothermal Preparation bismuth tungstate is characterized in that: the volumetric molar concentration of ammonium tungstate solution and bismuth nitrate solution is 0.001 ~ 0.5mol/L in the said step (1).The method of sol-gel of the present invention-Hydrothermal Preparation bismuth tungstate is characterized in that: the volumetric molar concentration of EDTA solution is 0.01 ~ 0.5mol/L in the said step (1).The method of sol-gel of the present invention-Hydrothermal Preparation bismuth tungstate is characterized in that: the acid in the said step (3) can be nitric acid, and alkali can be ammoniacal liquor.
The method of a kind of sol-gel-Hydrothermal Preparation indium doping bismuth tungstate; It is characterized in that: add indium nitrate in the sol-gel process in the preparation method of above-mentioned bismuth tungstate 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; Under stirring condition, in ammonium tungstate solution, bismuth nitrate solution and indium nitrate solution, add EDTA solution then respectively and form clear solution, wherein the add-on of EDTA is n (EDTA) in the ammonium tungstate solution: n (H
40N
10O
41W
12)=18:1, the add-on of EDTA is n (EDTA) in the bismuth nitrate solution: n (Bi (NO
3)
3)=1.5:1, the add-on of EDTA is n (EDTA) in the indium nitrate solution: 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, and the transparent mixed solution with gained keeps getting in 24 hours wet gel in 80 ℃ water-bath then, and wet gel is through 110 ℃ of dry xerogel that get; (3), the xerogel of step (2) gained is moved in the hydrothermal reaction kettle, using the pH value of acid or alkali conditioned reaction solution is 2 ~ 11, then 180 ~ 240 ℃ of maintenances after 6 ~ 36 hours, through coldly removing, filter, wash, obtain having after the drying Bi of high catalytic activity
2-
x In
x WO
6(0.01≤
x≤0.1) photocatalyst.The method of sol-gel of the present invention-Hydrothermal Preparation indium doping bismuth tungstate is characterized in that: the volumetric molar concentration of ammonium tungstate solution, bismuth nitrate solution and indium nitrate solution is 0.001 ~ 0.5mol/L in the said step (1).The method of sol-gel of the present invention-Hydrothermal Preparation indium doping bismuth tungstate is characterized in that: the volumetric molar concentration of said step (1) EDTA solution is 0.01 ~ 0.5mol/L.The method of sol-gel of the present invention-Hydrothermal Preparation bismuth tungstate is characterized in that: the acid in the said 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 bigger specific surface area and good photocatalytic activity.Method of the present invention has overcome in the existing preparation bismuth tungstate method that crystal grain is prone to reunite, difficult adulterated shortcoming, has prepared that particle diameter is little, the reunion degree is low, complete in crystal formation, has been prone to adulterated nanometer bismuth tungstate photocatalyst and the adulterated nanometer bismuth tungstate of indium photocatalyst.
Description of drawings
Fig. 1 is the bismuth tungstate (Bi of the embodiment of the invention 1 preparation
2WO
6) X-ray diffractogram.
Embodiment
Further describe the present invention in conjunction with following examples.Be noted that the present invention is not limited to following each embodiment.
Embodiment 1
(1), compound concentration is that 0.024mol/L bismuth nitrate solution and concentration are each 10mL of ammonium tungstate solution of 0.001mol/L; Under stirring condition, the EDTA solution that 3.6mL and 1.8mL concentration is 0.1mol/L joins respectively in bismuth nitrate solution and the ammonium tungstate solution;
(2), above-mentioned two kinds of clear solutions are mixed the back keeps getting in 24 hours wet gel, 110 ℃ of dry xerogel that get of wet gel warp in 60 ℃ water-bath;
(3), xerogel is moved in the hydrothermal reaction kettle, add the 50ml deionized water and, after 12 hours, naturally cool to room temperature 220 ℃ of maintenances then with the pH=2.0 of nitric acid conditioned reaction solution.To obtain the product spinning,, after 60 ℃ of vacuum-drying, obtain having the bismuth tungstate photocatalyst of high catalytic activity, can find out that from X ray diffracting spectrum its crystalline structure with bismuth tungstate is consistent with deionized water wash 3 times.
Embodiment 2
(1), compound concentration is that 0.24mol/L bismuth nitrate solution and concentration are each 10mL of ammonium tungstate solution of 0.01mol/L; Under stirring condition, the EDTA solution that respectively 7.2mL and 3.6mL concentration is 0.5mol/L joins in bismuth nitrate solution and the ammonium tungstate solution;
(2), above-mentioned two kinds of clear solutions are mixed the back keeps getting in 24 hours wet gel, 110 ℃ of dry xerogel that get of wet gel warp in 80 ℃ water-bath;
(3), xerogel is moved in the hydrothermal reaction kettle, add the 50ml deionized water and, after 6 hours, naturally cool to room temperature 240 ℃ of maintenances then with the pH=11.0 of ammoniacal liquor conditioned reaction solution.To obtain the product spinning,, after 60 ℃ of vacuum-drying, obtain having the bismuth tungstate photocatalyst of high catalytic activity with deionized water wash 3 times.
Embodiment 3
(1), compound concentration is that 0.12mol/L bismuth nitrate solution and concentration are each 10mL of ammonium tungstate solution of 0.005mol/L; Under stirring condition, the EDTA solution that respectively 3.6mL and 1.8mL concentration is 0.5mol/L joins in bismuth nitrate solution and the ammonium tungstate solution;
(2), above-mentioned two kinds of clear solutions are mixed the back keeps getting in 12 hours wet gel, 110 ℃ of dry xerogel that get of wet gel warp in 60 ℃ water-bath;
(3), xerogel is moved in the hydrothermal reaction kettle, add the 50ml deionized water and, after 36 hours, naturally cool to room temperature 180 ℃ of maintenances then with the pH=2.0 of nitric acid conditioned reaction solution.To obtain the product spinning,, after 60 ℃ of vacuum-drying, obtain having the bismuth tungstate photocatalyst of high catalytic activity with deionized water wash 3 times.
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 stirring condition, the EDTA solution that respectively 71.64mL, 0.36mL and 36mL concentration is 0.5mol/L joins in bismuth nitrate solution, indium nitrate solution and the ammonium tungstate solution;
(2), above-mentioned clear solution is mixed the back keeps getting in 24 hours wet gel, 110 ℃ of dry xerogel that get of wet gel warp in 80 ℃ water-bath;
(3), xerogel is moved in the hydrothermal reaction kettle, add the 100ml deionized water and, after 6 hours, naturally cool to room temperature 240 ℃ of maintenances then with the pH=11.0 of ammoniacal liquor conditioned reaction solution.To obtain the product spinning,, after 60 ℃ of vacuum-drying, obtain having the Bi of high catalytic activity with deionized water wash 3 times
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 stirring condition, the EDTA solution that 35.1mL, 0.9mL and 18mL concentration is 0.1mol/L joins respectively in Bismuth trinitrate, indium nitrate and the ammonium tungstate solution;
(2), above-mentioned clear solution is mixed the back keeps getting in 24 hours wet gel, 110 ℃ of dry xerogel that get of wet gel warp in 80 ℃ water-bath;
(3), xerogel is moved in the hydrothermal reaction kettle, add the 100ml deionized water and, after 12 hours, naturally cool to room temperature 220 ℃ of maintenances then with the pH=3.0 of nitric acid conditioned reaction solution.To obtain the product spinning,, after 60 ℃ of vacuum-drying, obtain having the Bi of high catalytic activity with deionized water wash 3 times
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 stirring condition, the EDTA solution that respectively 34.2mL, 1.8mL and 18mL concentration is 0.5mol/L joins in Bismuth trinitrate and the ammonium tungstate solution;
(2), above-mentioned clear solution is mixed the back keeps getting in 24 hours wet gel, 110 ℃ of dry xerogel that get of wet gel warp in 80 ℃ water-bath;
(3), xerogel is moved in the hydrothermal reaction kettle, add the 100ml deionized water and, after 36 hours, naturally cool to room temperature 180 ℃ of maintenances then with the pH=2.0 of nitric acid conditioned reaction solution.To obtain the product spinning,, after 60 ℃ of vacuum-drying, obtain having the Bi of high catalytic activity with deionized water wash 3 times
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 describes in the foregoing description and the specification sheets just explains principle of the present invention; Under the scope that does not break away from the principle of the invention, the present invention also has various changes and modifications, and these variations and improvement all fall in the scope of the present invention's protection.
Claims (8)
1. the method for sol-gel-Hydrothermal Preparation bismuth tungstate is characterized in that may further comprise the 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; Under stirring condition, in ammonium tungstate solution and bismuth nitrate solution, add EDTA solution then respectively and form clear solution, wherein the add-on of EDTA solution is n (EDTA) in the ammonium tungstate solution: n (H
40N
10O
41W
12)=18:1, the add-on of EDTA solution is n (EDTA) in the bismuth nitrate solution: n (Bi (NO
3)
3)=1.5:1; (2), with the clear solution of step (1) gained n (H in molar ratio
40N
10O
41W
12): n (Bi (NO
3)
3The mixed of)=1:24 is even, and the transparent mixed solution with gained keeps getting in 12-24 hour wet gel in 60-80 ℃ water-bath then, and wet gel is through 110 ℃ of dry xerogel that get; (3), the xerogel with step (2) gained moves in the hydrothermal reaction kettle; Using the pH value of acid or alkali conditioned reaction solution is 2 ~ 11; Then 180 ~ 240 ℃ keep 6 ~ 36 hours after, through coldly removing, filter, wash, obtain having after the drying bismuth tungstate photocatalyst of high catalytic activity.
2. the method for sol-gel according to claim 1-Hydrothermal Preparation bismuth tungstate is characterized in that: the volumetric molar concentration of ammonium tungstate solution and bismuth nitrate solution is 0.001 ~ 0.5mol/L in the said step (1).
3. the method for sol-gel according to claim 1-Hydrothermal Preparation bismuth tungstate is characterized in that: the volumetric molar concentration of said step (1) EDTA solution is 0.01 ~ 0.5mol/L.
4. the method for sol-gel according to claim 1-Hydrothermal Preparation bismuth tungstate is characterized in that: the acid in the said step (3) can be nitric acid, and alkali can be ammoniacal liquor.
5. the method for sol-gel-Hydrothermal Preparation indium doping bismuth tungstate; It is characterized in that: add indium nitrate in the sol-gel process in the preparation method of above-mentioned bismuth tungstate 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; Under stirring condition, in ammonium tungstate solution, bismuth nitrate solution and indium nitrate solution, add EDTA solution then respectively and form clear solution, wherein the add-on of EDTA is n (EDTA) in the ammonium tungstate solution: n (H
40N
10O
41W
12)=18:1, the add-on of EDTA is n (EDTA) in the bismuth nitrate solution: n (Bi (NO
3)
3)=1.5:1, the add-on of EDTA is n (EDTA) in the indium nitrate solution: 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, and the transparent mixed solution with gained keeps getting in 24 hours wet gel in 80 ℃ water-bath then, and wet gel is through 110 ℃ of dry xerogel that get; (3), the xerogel of step (2) gained is moved in the hydrothermal reaction kettle, using the pH value of acid or alkali conditioned reaction solution is 2 ~ 11, then 180 ~ 240 ℃ of maintenances after 6 ~ 36 hours, through coldly removing, filter, wash, obtain having after the drying Bi of high catalytic activity
2-
x In
x WO
6(0.01≤
x≤0.1) photocatalyst.
6. the method for sol-gel according to claim 5-Hydrothermal Preparation indium doping bismuth tungstate is characterized in that: the volumetric molar concentration of ammonium tungstate solution, bismuth nitrate solution and indium nitrate solution is 0.001 ~ 0.5mol/L in the said step (1).
7. the method for sol-gel according to claim 5-Hydrothermal Preparation indium doping bismuth tungstate is characterized in that: the volumetric molar concentration of said step (1) EDTA solution is 0.01 ~ 0.5mol/L.
8. the method for sol-gel according to claim 5-Hydrothermal Preparation indium doping bismuth tungstate, it is characterized in that: the acid in the said step (3) can be nitric acid, alkali can be ammoniacal liquor.
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| CN103611528A (en) * | 2013-12-05 | 2014-03-05 | 河南师范大学 | Method for preparing bismuth tungstate catalyst by taking egg white as template |
| CN103611559A (en) * | 2013-12-05 | 2014-03-05 | 河南师范大学 | Bi2WO6-SrTaO2N composite photocatalyst and preparation method thereof |
| CN103623811A (en) * | 2013-09-12 | 2014-03-12 | 陕西科技大学 | In-Bi2WO6 photocatalyst with low electron hole recombination rate and preparation method thereof |
| CN103818962A (en) * | 2013-12-30 | 2014-05-28 | 烟台佳隆纳米产业有限公司 | Preparation method of cesium tungsten oxide ultrafine powder |
| CN105679546A (en) * | 2016-01-18 | 2016-06-15 | 黑龙江大学 | InWO4:Eu<3+>/TiO2 composite photo anode and preparation method thereof |
| CN106732534A (en) * | 2016-11-29 | 2017-05-31 | 辽宁大学 | A kind of infrared ray excited bismuth tungstate photocatalyst and preparation method thereof |
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| CN103623811A (en) * | 2013-09-12 | 2014-03-12 | 陕西科技大学 | In-Bi2WO6 photocatalyst with low electron hole recombination rate and preparation method thereof |
| 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 |
| CN103611528A (en) * | 2013-12-05 | 2014-03-05 | 河南师范大学 | Method for preparing bismuth tungstate catalyst by taking egg white as template |
| CN103611559A (en) * | 2013-12-05 | 2014-03-05 | 河南师范大学 | Bi2WO6-SrTaO2N composite photocatalyst and preparation method thereof |
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| 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 |
| CN103818962A (en) * | 2013-12-30 | 2014-05-28 | 烟台佳隆纳米产业有限公司 | Preparation method of cesium tungsten oxide ultrafine powder |
| 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 |
| CN105679546A (en) * | 2016-01-18 | 2016-06-15 | 黑龙江大学 | InWO4:Eu<3+>/TiO2 composite photo anode and preparation method thereof |
| CN106732534A (en) * | 2016-11-29 | 2017-05-31 | 辽宁大学 | A kind of infrared ray excited bismuth tungstate photocatalyst 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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