CN100566821C - A kind of preparation method who contains the composite photocatalyst material of rare earth element - Google Patents

A kind of preparation method who contains the composite photocatalyst material of rare earth element Download PDF

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CN100566821C
CN100566821C CNB2008100327747A CN200810032774A CN100566821C CN 100566821 C CN100566821 C CN 100566821C CN B2008100327747 A CNB2008100327747 A CN B2008100327747A CN 200810032774 A CN200810032774 A CN 200810032774A CN 100566821 C CN100566821 C CN 100566821C
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composite photocatalyst
rare earth
preparation
photocatalyst material
earth element
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CN101219375A (en
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闫冰
李灵芝
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Tongji University
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Abstract

The invention belongs to the catalysis material technical field, be specifically related to a kind of preparation method who contains the composite photo-catalyst of rare earth element, the chemical formula of this composite photocatalyst material is: Y XBi 1-XVO 4/ Bi 2O 3, X＜0.51 wherein, concrete preparation process is as follows: with Y 2O 3, Bi (NO 3) 35H 2O, NH 4VO 3Be raw material, adopt hydro-thermal reaction and solid reaction process under different temperatures, to synthesize stable chemical performance, the strong catalysis material Y that absorbs is arranged at visible light XBi 1-XVO 4/ Bi 2O 3, (X＜0.51), it can be decomposing organic pollutant under the radiation of visible light (as rhodamine B), mild condition required for the present invention, and make organic pollution (as rhodamine B) degraded thoroughly.This method is workable, favorable reproducibility, and products obtained therefrom steady quality, and catalytic effect is good, can be used for environmental pollution improvement.

Description

A kind of preparation method who contains the composite photocatalyst material of rare earth element
Technical field
The invention belongs to the catalysis material technical field, be specifically related to a kind of preparation method who contains the composite photo-catalyst of rare earth element.
Background technology
U.S. Carey in 1976 is about the report of photocatalysis Decomposition biphenyl and biphenylene oxide, is considered to photocatalysis in the initiative research work of eliminating aspect the environmental contaminants.Henceforth, the research of Treatment by Photocatalysis Oxidation organic pollution is increasing.Utilize photocatalysis technology the organic pollution oxidation Decomposition can be become inorganic matter, course of reaction is expressed as follows:
Organic pollution+O 2→ CO 2+ H 2O+......
Reaction system is converted into chemical energy with the luminous energy that absorbs under photocatalysis, many being reflected under the comparatively gentle condition of generally being difficult to realize can be carried out smoothly, although the reaction mechanism of its complexity is unclear by understanding as yet at present, but the research of application facet has been made brilliant achievements, and has shown multiphase photocatalysis is administered the field at organic pollution applications well prospect.
BiVO 4Obtaining some application aspect the degraded mineralising organic pollution, but its photocatalysis performance is subjected to the influence of its crystal formation.The BiVO of monocline phase (monoclinic) 4Stronger photocatalytic activity is arranged, and the BiVO of cubic phase (tetragonal) 4Almost do not have.For improving the BiVO of monocline phase 4Catalytic activity, it is mixed or compound.
At present, normal adopt Ag/BiVO arranged 4, Pd/BiVO 4, Co 3O 4/ BiVO 4, wait composite photo-catalyst, but needed experiment condition is than higher in the building-up process, use and be subjected to certain limitation.Adopt rare earth compound and BiVO simultaneously 4The research of compound visible light catalytic material is not a lot, and is by discovering that compound catalysis material afterwards under radiation of visible light, has tangible light-catalysed activity, more thorough to organic pollutant degradation.China's rare earth resources is abundant, adopts rare earth compound and BiVO 4Compound preparation visible light catalytic material has very big application prospect.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who contains the composite photocatalyst material of rare earth element.
The preparation method of the composite photocatalyst material that contains rare earth element that the present invention proposes, the chemical formula of this composite photocatalyst material is: Y XBi 1-XVO 4/ Bi 2O 3, X＜0.51 wherein, concrete steps are as follows:
(1) raw material proportioning: with Y 2O 3Be dissolved in nitric acid and make Y (NO 3) 3, with Bi (NO 3) 35H 2O and NH 4VO 3For raw material is configured to the solution that molar concentration is 0.4-1.0mol/l respectively, be that 1: 4: 5～1: 1: 2 ratio is mixed three kinds of solution according to the mol ratio of Y, Bi and V, the pH value of regulating mixture is 6-7, at room temperature stirs 0.5～1h, and it is fully reacted;
(2) hydrothermal synthesis reaction: the mixture of step (1) gained is placed the polytetrafluoroethylene (PTFE) reactor, under 150～190 ℃ of temperature, react 24～72h;
(3) with pure water washing step (2) gained solid product, drying promptly gets Y XBi 1-XVO 4, X＜0.51 wherein;
(4) roasting: with Bi (NO 3) 35H 2O promptly gets product B i at roasting temperature 2～6h of 500～700 ℃ 2O 3
(5) be that 3: 1～1: 2 ratio is mixed with step (3) products therefrom and step (4) products therefrom according to mass ratio, promptly get required product.
Among the present invention, adopt ammoniacal liquor to regulate the pH value of mixture in the step (1).
Among the present invention, the described baking temperature of step (3) is 60-70 ℃.
What the present invention prepared has the strong composite photocatalyst material Y that absorbs at visible region XBi 1-XVO 4/ Bi 2O 3, (X＜0.51), its catalytic effect can adopt rhodamine B to verify.
Mild condition required for the present invention, and make organic pollutant degradation thorough.This method is workable, favorable reproducibility, and products obtained therefrom steady quality, and catalytic effect is good.
Description of drawings
Fig. 1 is the embodiment of the invention 1 products therefrom Y 0.33Bi 0.67VO 4/ Bi 2O 3The X-ray diffraction spectrogram.Wherein, curve a is Y 0.33Bi 0.67VO 4The X-ray diffraction spectrogram, curve b is Bi 2O 3The X-ray diffraction spectrogram.
Fig. 2 is the embodiment of the invention 1 products therefrom Y 0.33Bi 0.67VO 4/ Bi 2O 3The UV, visible light spectrogram that diffuses.Wherein, curve a is Y 0.33Bi 0.67VO 4The UV, visible light spectrogram that diffuses, curve b is Bi 2O 3The UV, visible light spectrogram that diffuses.
Fig. 3 is the embodiment of the invention 1 products therefrom Y 0.33Bi 0.67VO 4/ Bi 2O 3Sem photograph.Wherein, curve a is Y 0.33Bi 0.67VO 4Sem photograph, curve b is Bi 2O 3Sem photograph.
Fig. 4 is with the embodiment of the invention 1 products therefrom Y 0.33Bi 0.67VO 4With Bi 2O 3Join in the rhodamine B solution according to the different quality ratio, under radiation of visible light, rhodamine B concentration curve figure in 6h.Wherein (a) is Y 0.33Bi 0.67VO 4With Bi 2O 3Mass ratio be 3: 1, (b) be Y 0.33Bi 0.67VO 4With Bi 2O 3Mass ratio be 3: 2, (c) be Y 0.33Bi 0.67VO 4With Bi 2O 3Mass ratio be 1: 1, (d) be Y 0.33Bi 0.67VO 4With Bi 2O 3Mass ratio be 3: 4, (e) Y 0.33Bi 0.67VO 4With Bi 2O 3Mass ratio be 3: 5.
The specific embodiment
Further specify the present invention below by embodiment, but protection scope of the present invention is not limited to these embodiment.
Embodiment 1
With Bi (NO 3) 35H 2O and NH 4VO 3For raw material is prepared the Bi (NO that molar concentration is 0.40mol/l respectively 3) 3With molar concentration be the NH of 0.60mol/l 4VO 3Solution.Take by weighing the Y of 0.113g 2O 3Be dissolved in nitric acid and make Y (NO 3) 3Solution is to the Bi (NO that wherein adds the 5.00ml that has prepared 3) 3The NH of solution and 5.00ml 4VO 3Solution, the pH value of regulating mixture with ammoniacal liquor is 7, at room temperature stirs 1h, and it is fully mixed.The mixture of gained is packed in the polytetrafluoroethylene (PTFE) reactor, obtaining suspension behind the reaction 48h under 160 ℃ of conditions, cooled and filtered obtains solid, with pure water cyclic washing gained solid product, place then under 70 ℃ of conditions of baking oven dry, Y 0.33Bi 0.67VO 4With 2.425gBi (NO 3) 35H 2O is 600 ℃ roasting temperature 4 hours, product B i 2O 3According to different quality ratio 3: 1,3: 2,3: 3, mix the Y of preparation before this at 3: 4.3: 5 0.33Bi 0.67VO 4And Bi 2O 3, promptly obtain required product.Ratio according to 1mg/ml joins products obtained therefrom in the rhodamine B of 100 milliliters of 10mol/l, and with the whole system 6h of radiation of visible light, experiment shows that the gained mixture all shows higher activity to the photocatalysis decolouring of rhodamine B.
Embodiment 2
With Bi (NO 3) 35H 2O and NH 4VO 3For raw material is prepared the Bi (NO that molar concentration is 1.00mol/l respectively 3) 3With molar concentration be the NH of 1.00mol/l 4VO 3Solution.Take by weighing the Y of 0.226g 2O 3Be dissolved in nitric acid and make Y (NO 3) 3The heating evaporate to dryness is to the Bi (NO that wherein adds the 8.00ml that has prepared 3) 3NH with 10.00ml 4VO 3Solution, the pH value of regulating mixture with ammoniacal liquor is 6, at room temperature stirs 0.7h, and it is fully mixed.The mixture of gained is packed in the polytetrafluoroethylene (PTFE) reactor, obtaining suspension behind the reaction 36h under 180 ℃ of conditions, cooled and filtered obtains solid.With pure water cyclic washing gained solid product, place drying under 60 ℃ of conditions of baking oven then, get Y 0.3Bi 0.7VO 4With 2.425gBi (NO 3) 35H 2O is 700 ℃ roasting temperature 2 hours, product B i 2O 3According to different quality ratio 3: 1,3: 2,3: 3, mix the Y of preparation before this at 3: 4.3: 6 0.25Bi 0.75VO 4And Bi 2O 3, promptly obtain required product.Ratio according to 1mg/ml joins products obtained therefrom in the rhodamine B of 100 milliliters of 10mol/l, and with the whole system 6h of radiation of visible light, experiment shows that the gained mixture all shows higher activity to the photocatalysis decolouring of rhodamine B.
Embodiment 3
With Bi (NO 3) 35H 2O and NH 4VO 3For raw material is prepared the Bi (NO that molar concentration is 1.00mol/l respectively 3) 3With molar concentration be the NH of 1.00mol/l 4VO 3Solution.Take by weighing the Y of 0.226g 2O 3Be dissolved in nitric acid and make Y (NO 3) 3The heating evaporate to dryness is to the Bi (NO that wherein adds the 2.00ml that has prepared 3) 3NH with 4.00ml 4VO 3Solution, the pH value of regulating mixture with ammoniacal liquor is 6, at room temperature stirs 0.5h, and it is fully mixed.The mixture of gained is packed in the polytetrafluoroethylene (PTFE) reactor, obtaining suspension behind the reaction 72h under 150 ℃ of conditions, cooled and filtered obtains solid.With pure water cyclic washing gained solid product, place drying under 65 ℃ of conditions of baking oven then, get Y 0.25Bi 0.75VO 4With 2.425gBi (NO 3) 35H 2O is 500 ℃ roasting temperature 6 hours, product B i 2O 3According to different quality ratio 3: 1,3: 2,3: 3, mix the Y of preparation before this at 3: 4.3: 6 0.5Bi 0.5VO 4And Bi 2O 3, promptly obtain required product.
Embodiment 4
With Bi (NO 3) 35H 2O and NH 4VO 3Preparing molar concentration respectively for raw material is 1.00mol/l Bi (NO 3) 3With molar concentration be the NH of 1.00mol/l 4VO 3Solution.Take by weighing the Y of 0.113g 2O 3Be dissolved in nitric acid and make Y (NO 3) 3The heating evaporate to dryness is to the Bi (NO that wherein adds the 3.00ml that has prepared 3) 3NH with 4.00ml 4VO 3Solution, the pH value of regulating mixture with ammoniacal liquor is 7, at room temperature stirs 1h, and it is fully mixed.The mixture of gained is packed in the polytetrafluoroethylene (PTFE) reactor, obtaining suspension behind the reaction 48h under 170 ℃ of conditions, cooled and filtered obtains solid.With pure water cyclic washing gained solid product, place drying under 70 ℃ of conditions of baking oven then, get Y 0.33Bi 0.67VO 4With 2.425gBi (NO 3) 35H 2O is 600 ℃ roasting temperature 4 hours, product B i 2O 3According to different quality ratio 3: 1,3: 2,3: 3, mix the Y of preparation before this at 3: 4.3: 5 0.33Bi 0.67VO 4And Bi 2O 3, promptly obtain required product.Ratio according to 1mg/ml joins products obtained therefrom in the rhodamine B of 10mol/l, and with the whole system 6h of radiation of visible light, experiment shows that the gained mixture all shows higher activity to the photocatalysis decolouring of rhodamine B.
Embodiment 5
With Bi (NO 3) 35H 2O and NH 4VO 3For raw material is prepared the Bi (NO that molar concentration is 0.40mol/l respectively 3) 3With molar concentration be the NH of 0.60mol/l 4VO 3Solution.Take by weighing the Y of 0.226g 2O 3Be dissolved in nitric acid and make Y (NO 3) 3The heating evaporate to dryness is to the Bi (NO that wherein adds the 10.00.ml that has prepared 3) 3NH with 10.00ml 4VO 3Solution, the pH value of regulating mixture with ammoniacal liquor is 7, at room temperature stirs 0.8h, and it is fully mixed.The mixture of gained is packed in the polytetrafluoroethylene (PTFE) reactor, obtain suspension in reaction under 170 ℃ of conditions after 52 hours, cooled and filtered obtains solid.With pure water cyclic washing gained solid product, place drying under 70 ℃ of conditions of baking oven then, get Y 0.3Bi 0.7VO 4With 2.425gBi (NO 3) 35H 2O is 550 ℃ roasting temperature 5 hours, product B i 2O 3According to different quality ratio 3: 1,3: 2,3: 3, mix the Y of preparation before this at 3: 4.3: 5 0.4Bi 0.6VO 4And Bi 2O 3, promptly obtain required product.Ratio according to 1mg/ml joins products obtained therefrom in the rhodamine B of 100 milliliters of 10mol/l, and with the whole system 6h of radiation of visible light, experiment shows that the gained mixture all shows higher activity to the photocatalysis decolouring of rhodamine B.
Embodiment 6
With Bi (NO 3) 35H 2O and NH 4VO 3For raw material is prepared the Bi (NO that molar concentration is 0.40mol/l respectively 3) 3With molar concentration be the NH of 0.60mol/l 4VO 3Solution.Take by weighing the Y of 0.068g 2O 3Be dissolved in nitric acid and make Y (NO 3) 3The heating evaporate to dryness is to the Bi (NO that wherein adds the 6.00ml that has prepared 3) 3NH with 5.00ml 4VO 3Solution, the pH value of regulating mixture with ammoniacal liquor is 7, at room temperature stirs 0.9h, and it is fully mixed.The mixture of gained is packed in the polytetrafluoroethylene (PTFE) reactor, obtaining suspension behind the reaction 36h under 180 ℃ of conditions, cooled and filtered obtains solid.With pure water cyclic washing gained solid product, place drying under 70 ℃ of conditions of baking oven then, get Y 0.25Bi 0.75VO 4With 2.425gBi (NO 3) 35H 2O is 700 ℃ roasting temperature 2 hours, product B i 2O 3According to different quality ratio 3: 1,3: 2,3: 3, mix the Y of preparation before this at 3: 4.3: 5 0.25Bi 0.75VO 4And Bi 2O 3, promptly get required product.Ratio according to 1mg/ml joins products obtained therefrom in the rhodamine B of 100 milliliters of 10mol/l, and with the whole system 6h of radiation of visible light, experiment shows that the gained mixture all shows higher activity to the photocatalysis decolouring of rhodamine B.

Claims (4)

1, a kind of preparation method who contains the composite photocatalyst material of rare earth element is characterized in that the chemical formula of this composite photocatalyst material is: Y XBi 1-XVO 4/ Bi 2O 3, wherein X is 0.25-0.5, concrete steps are as follows:
(1) raw material proportioning: with Y 2O 3Be dissolved in nitric acid and make Y (NO 3) 3, with Bi (NO 3) 35H 2O and NH 4VO 3For raw material is configured to the solution that molar concentration is 0.4-1.0mol/L respectively, be that 1: 4: 5～1: 1: 2 ratio is mixed three kinds of solution according to the mol ratio of Y, Bi and V, the pH value of regulating mixture is 6-7, at room temperature stirs 0.5～1h, and it is fully reacted;
(2) hydrothermal synthesis reaction: the mixture of step (1) gained is placed the polytetrafluoroethylene (PTFE) reactor, under 150～190 ℃ of temperature, react 24～72h;
(3) filtration washing: with pure water washing step (2) gained solid product, drying promptly gets Y XBi 1-XVO 4, wherein X is 0.25-0.5;
(4) roasting: with Bi (NO 3) 35H 2O promptly gets product B i at roasting temperature 2～6h of 500～700 ℃ 2O 3
(5) be that 3: 1～1: 2 ratio is mixed with step (3) products therefrom and step (4) products therefrom according to mass ratio, promptly get required product.
2, the preparation method who contains the composite photocatalyst material of rare earth element according to claim 1 is characterized in that adopting in the step (1) ammoniacal liquor to regulate the pH value of mixture.
3, the preparation method who contains the composite photocatalyst material of rare earth element according to claim 1 is characterized in that the described baking temperature of step (3) is 60-70 ℃.
4, the preparation method who contains the composite photocatalyst material of rare earth element according to claim 1 is characterized in that the catalytic effect of gained composite photocatalyst material adopts rhodamine B to verify.
CNB2008100327747A 2008-01-17 2008-01-17 A kind of preparation method who contains the composite photocatalyst material of rare earth element Expired - Fee Related CN100566821C (en)

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CN101690891B (en) * 2009-09-25 2011-07-27 南京大学 Synthetic method of visible light catalyst SnWO4
CN102658116B (en) * 2012-04-14 2014-01-01 吉林大学 Rare earth element-doped bismuth oxide photocatalyst and preparation method thereof
CN103240073B (en) * 2013-04-26 2015-01-28 南京信息工程大学 Zn<2+>-doped BiVO4 visible-light-driven photocatalyst and preparation method thereof
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