CN105032399B - A kind of pucherite tin oxide composite photo-catalyst and its preparation method and application - Google Patents
A kind of pucherite tin oxide composite photo-catalyst and its preparation method and application Download PDFInfo
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- CN105032399B CN105032399B CN201510501080.3A CN201510501080A CN105032399B CN 105032399 B CN105032399 B CN 105032399B CN 201510501080 A CN201510501080 A CN 201510501080A CN 105032399 B CN105032399 B CN 105032399B
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Abstract
The invention discloses a kind of pucherite tin oxide composite photo-catalyst and its preparation method and application, comprise the following steps：(1) stannic chloride and bismuth nitrate are dissolved in salpeter solution, after being sufficiently stirred for, are configured to acidic mixed solution；Take ammonium metavanadate to be dissolved in sodium hydroxide solution, after being sufficiently stirred for, be configured to alkaline sodium vanadate solution；(2) under agitation, above-mentioned mixed solution is added dropwise in sodium vanadate solution, makes its generation bright yellow solution；(3) toward alkaline solution in bright yellow solution, is added dropwise over, adjustment pH value is more than 8, and mixed liquor is carried out hydro-thermal reaction by ultrasonic vibration；(4) treat that hydrothermal product is cooled to room temperature, cleaned with deionized water, it is pucherite tin oxide composite photo-catalyst that gained powder is dried after filtering.Invention preparation method is simple, with low cost, reproducible, can well meet volume production requirement；Prepared catalyst can carry out Methyl blueness under visible light.
Description
Technical field
The present invention relates to inorganic nano photocatalyst material field, more particularly to a kind of composite photo-catalyst and its preparation side
Method.
Background technology
In in the past few decades, photocatalysis technology has been widely used for degrade toxic organic pollutant and photodissociation aquatic products
The field of hydrogen energy source.TiO2Because its high chemical stability, low cost, nontoxicity and turn into current most widely used semiconductor
Material.But, TiO2But it is restricted in actual applications, because TiO2Band-gap energy be 3.2eV, this means that TiO2
Ultraviolet light can only be utilized, and ultraviolet light only accounts for 4% in sun emission spectrum, remaining other solar spectrals cannot fill
The utilization for dividing.Therefore, many scholars are devoted to developing the catalyst material of visible optical drive in the last few years, and be is exactly fully high
The utilization solar energy of effect.
In the last few years, band-gap energy only had the monoclinic crystal pucherite (m-BiVO of 2.4eV4) as it is a kind of it is very promising can
See that optical response semiconductor material obtains the attention of more and more scholars.Many researchs find BiVO4Have under visible light conditions
Extraordinary photoresponse ability, some organic pollutants while it can also effectively degrade.But simple pucherite is used as light
Catalyst is also faced with some problems, for example：Specific surface area is too small, and adsorption capacity is poor, and photo-generated carrier is difficult to separate,
Electron hole pair is easily compound etc., and these defects all limit the photocatalysis performance of pucherite.
The content of the invention
The problem to be solved in the present invention is that traditional pucherite monolithic catalyst has specific surface area too small, energy of adsorption
Power is poor, and photo-generated carrier is difficult to separate, and the easy defect such as compound of electron hole pair, these defects all limit pucherite
Photocatalysis performance, construct it is a kind of electric charge can be promoted to efficiently separate, the tin oxide nano particle with highlight catalytic active is repaiied
Decorations composite bismuth vanadium photocatalyst and preparation method thereof, tin oxide nano particle is discretely compound in vanadium in the composite photo-catalyst
The surface of sour bismuth, is conducive to exposing the tin oxide-pucherite boundary of high activity, in fields such as environment pollution control, the energy
It is with a wide range of applications；The preparation method of the composite photo-catalyst is simple, with low cost, reproducible simultaneously, can be very
Volume production requirement is met well.
Technical scheme is as follows：
A kind of preparation method of pucherite-tin oxide composite photo-catalyst, comprises the following steps：
(1) stannic chloride and bismuth nitrate are dissolved in salpeter solution, after being sufficiently stirred for, are configured to acidic mixed solution；Take with
The ammonium metavanadate of the identical molal quantity of bismuth nitrate is dissolved in sodium hydroxide solution, after being sufficiently stirred for, is configured to alkaline sodium vanadate solution；
(2) under agitation, the mixed solution of step (1) is added dropwise in sodium vanadate solution, makes its generation bright orange
Color solution；
(3) toward in bright yellow solution, being added dropwise over alkaline solution, adjustment pH value is more than 8, more than ultrasonic vibration 20min,
Mixed liquor is carried out into hydro-thermal reaction；
(4) treat that hydrothermal product is cooled to room temperature, cleaned with deionized water, after filtering dry gained powder be pucherite-
Tin oxide composite photo-catalyst.
The condition of the hydro-thermal reaction be 120~180 DEG C under the conditions of, react 20~30h.
The condition of the hydro-thermal reaction be 150 DEG C under the conditions of, react 24h.
The mol ratio of stannic chloride and bismuth nitrate described in step (1) is (2~4):7.
The mol ratio of the stannic chloride and bismuth nitrate is 3:7.
Alkaline solution described in step (3) is sodium hydroxide solution, and pH is adjusted to 10.
The ultrasonic vibration time described in step (4) is 30min；To be placed in baking oven, treatment temperature is the drying condition
60 DEG C, process time is 24h.
The concentration of step (1) described nitric acid is 4M, and the concentration of sodium hydroxide solution is 4M.
Pucherite obtained in the above method-tin oxide composite photo-catalyst, for carrying out photocatalytic degradation under visible light
Methyl blue.
Compared with prior art, the invention has the advantages that：
(1) present invention construct a kind of discrete composite photo-catalyst for being compound in pucherite of tin oxide nano particle, this with
Traditional block pucherite monolithic catalyst is compared, and composite catalyst possesses bigger specific surface area, is conducive to improving catalyst
Catalysis activity；
(2) pucherite that realizes of the invention is compound with tin oxide, forms pucherite-tin oxide heterogeneous structure, this
Structure is very beneficial for the separation of photo-generated carrier, reduces the combined efficiency of electron hole pair, improves the catalysis of catalyst
Performance；And due to the presence of heterojunction structure, photo-generated carrier efficiently can be transferred to catalyst material from heterostructure interface
Expect above the matrix of adsorption, so that a quick oxidation-reduction process can be more prone to realize.
(3) preparation method of the present invention is simple, the requirement to equipment is low, with low cost, reproducible, can meet well
Volume production requirement；The characteristics of present invention is based on composite, both pucherite and tin oxide are combined, can be in visible ray
Under, carry out Methyl blueness (MB).
Brief description of the drawings
Fig. 1 is the XRD spectrum of the pucherite-tin oxide composite photo-catalyst prepared by embodiment 1；
Fig. 2 is pucherite-tin oxide composite photo-catalyst prepared by embodiment 1 photocatalytic degradation methyl under visible light
Blue design sketch, is referenced as blank, pure tin oxide and pucherite.
Specific embodiment
The present invention is more specifically described in detail with reference to specific embodiment, but embodiments of the present invention are not limited
In this, for especially not dated technological parameter, can refer to routine techniques is carried out.
Embodiment 1
Under normal temperature and pressure, the Bi (NO of 3.39g are weighed3)3·5H2The SnCl of O and 1.05g4.5H2O powder in beaker A, plus
Enter the nitric acid that 20mL concentration is 4M, settled solution is obtained after being sufficiently stirred for；The another NH weighed with 0.82g4VO3In beaker B, plus
Enter the NaOH that 20mL concentration is 4M, settled solution is obtained after being sufficiently stirred for；Then in the case of quick stirring, by solution A by
It is added dropwise in B solution, obtains the solution of glassy yellow, it is the NaOH solution of 1M to add concentration, and adjustment pH value is 10, ultrasonic vibration
After 30min, the bright yellow solution is transferred in the hydrothermal reaction kettle of 100mL, under the conditions of 150 DEG C, hydro-thermal reaction 24h.Treat
Room temperature is cooled to, after product is cleaned for several times with deionized water, is placed in 60 DEG C of baking oven and is processed 24h.Room temperature is cooled to, will
Gained powder is finely ground with agate mortar, obtains final product pucherite-tin oxide composite catalyst powder 2.54g.
Embodiment 2
Under normal temperature and pressure, the Bi (NO of 3.41g are weighed3)3·5H2The SnCl of O and 1.06g4.5H2O powder in beaker A, plus
Enter the nitric acid that 20mL concentration is 4M, settled solution is obtained after being sufficiently stirred for；The another NH weighed with 0.83g4VO3In beaker B, plus
Enter the NaOH that 20mL concentration is 4M, settled solution is obtained after being sufficiently stirred for；Then in the case of quick stirring, by solution A by
It is added dropwise in B solution, obtains the solution of glassy yellow, it is the NaOH solution of 1M to add concentration, and adjustment pH value is 10, ultrasonic vibration
After 30min, the bright yellow solution is transferred in the hydrothermal reaction kettle of 100mL, under the conditions of 150 DEG C, hydro-thermal reaction 24h.Treat
Room temperature is cooled to, after product is cleaned for several times with deionized water, is placed in 60 DEG C of baking oven and is processed 24h.Room temperature is cooled to, will
Gained powder is finely ground with agate mortar, obtains final product pucherite-tin oxide composite catalyst powder 2.41g.
Embodiment 3
Under normal temperature and pressure, the Bi (NO of 6.79g are weighed3)3·5H2The SnCl of O and 2.11g4.5H2O powder in beaker A, plus
Enter the nitric acid that 20mL concentration is 4M, settled solution is obtained after being sufficiently stirred for；The another NH weighed with 1.65g4VO3In beaker B, plus
Enter the NaOH that 20mL concentration is 4M, settled solution is obtained after being sufficiently stirred for；Then in the case of quick stirring, by solution A by
It is added dropwise in B solution, obtains the solution of glassy yellow, it is the NaOH solution of 1M to add concentration, and adjustment pH value is 10, ultrasonic vibration
After 30min, the bright yellow solution is transferred in the hydrothermal reaction kettle of 100mL, under the conditions of 150 DEG C, hydro-thermal reaction 24h.Treat
Room temperature is cooled to, after product is cleaned for several times with deionized water, is placed in 60 DEG C of baking oven and is processed 24h.Room temperature is cooled to, will
Gained powder is finely ground with agate mortar, obtains final product pucherite-tin oxide composite catalyst powder 4.98g.
Claims (9)
1. the preparation method of a kind of pucherite-tin oxide composite photo-catalyst, it is characterised in that comprise the following steps：
(1) stannic chloride and bismuth nitrate are dissolved in salpeter solution, after being sufficiently stirred for, are configured to acidic mixed solution；Take and nitric acid
The ammonium metavanadate of the identical molal quantity of bismuth is dissolved in sodium hydroxide solution, after being sufficiently stirred for, is configured to alkaline sodium vanadate solution；It is described
The mol ratio of stannic chloride and bismuth nitrate is (2~4):7；
(2) under agitation, the mixed solution of step (1) is added dropwise in sodium vanadate solution, makes its generation glassy yellow molten
Liquid；
(3) toward in bright yellow solution, being added dropwise over alkaline solution, adjustment pH value is more than 8, more than ultrasonic vibration 20min, will be mixed
Closing liquid carries out hydro-thermal reaction；
(4) treat that hydrothermal product is cooled to room temperature, cleaned with deionized water, it is pucherite-oxidation that gained powder is dried after filtering
Tin composite photo-catalyst.
2. preparation method according to claim 1, it is characterised in that the condition of the hydro-thermal reaction is 120~180 DEG C of bars
Under part, 20~30h is reacted.
3. preparation method according to claim 2, it is characterised in that the condition of the hydro-thermal reaction is under the conditions of 150 DEG C,
Reaction 24h.
4. the preparation method according to claim 1 or 2 or 3, it is characterised in that the mol ratio of the stannic chloride and bismuth nitrate
It is 3:7.
5. the preparation method according to claim 1 or 2 or 3, it is characterised in that alkaline solution described in step (3) is hydrogen
Sodium hydroxide solution, pH is adjusted to 10.
6. the preparation method according to claim 1 or 2 or 3, it is characterised in that ultrasonic vibration time described in step (3)
It is 30min；To be placed in baking oven, treatment temperature is 60 DEG C to step (4) described drying condition, and process time is 24h.
7. the preparation method according to claim 1 or 2 or 3, it is characterised in that the concentration of step (1) described nitric acid is 4M,
The concentration of sodium hydroxide solution is 4M.
8. pucherite obtained in any one of claim 1~7 methods described-tin oxide composite photo-catalyst.
9. the application of composite photo-catalyst described in claim 8, it is characterised in that the composite photo-catalyst is used in visible ray
Under carry out Methyl blueness.
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| CN111979561B (en) * | 2019-05-21 | 2022-08-26 | 南京理工大学 | SnOx/BiVO 4 Electrode, preparation method thereof and application of electrode in photoelectrocatalysis hydrogen peroxide synthesis |
| CN110935437A (en) * | 2019-12-18 | 2020-03-31 | 兰州大学 | Synthetic method of Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water |
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| CN103464138A (en) * | 2013-08-15 | 2013-12-25 | 陕西科技大学 | Ytterbium doped bismuth vanadate visible light photocatalyst, and preparation method and application thereof |
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