CN107570141A - A kind of activated carbon supported bismuth tungstate photocatalyst and preparation method and application - Google Patents
A kind of activated carbon supported bismuth tungstate photocatalyst and preparation method and application Download PDFInfo
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- CN107570141A CN107570141A CN201710958575.8A CN201710958575A CN107570141A CN 107570141 A CN107570141 A CN 107570141A CN 201710958575 A CN201710958575 A CN 201710958575A CN 107570141 A CN107570141 A CN 107570141A
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Abstract
The invention discloses a kind of activated carbon supported bismuth tungstate photocatalyst and preparation method and application, wherein：The supported bismuth tungstate photocatalyst is by the way that bismuth tungstate and carrier granular activated carbon are combined；The present invention is prepared for activated carbon supported bismuth tungstate photocatalyst by colloidal sol-gel-roasting technology, and the present invention characterizes structure, the pattern of material, and have studied its visible light photocatalytic degradation Microcystin MC LR activity.As a result show, bismuth tungstate has successfully been loaded on activated carbon, and improves visible light photocatalysis active.Of the present invention to prepare that material is nontoxic and cost is low, operating method simplicity is easy to control.
Description
Technical field
The invention belongs to inorganic environment-friendly catalysis material technical field, more particularly to a kind of activated carbon supported bismuth tungstate light is urged
Agent and preparation method and application.
Background technology
Water pollution is the important environmental problem faced at present, efficient, pollution-free, the inexpensive pollution control of water of exploitation
Technology be facing mankind significant challenge, and problem in the urgent need to address.Go in water removal to pollute using photocatalysis technology
Thing is one of current most active research field.Early stage most study is TiO2Photochemical catalyst, it has, and catalytic activity is high, surely
Qualitative good, price is low, nontoxic to wait premium properties.But TiO2Energy gap is about 3.2eV, and only wavelength is less than 387nm purple
Outer light can just excite its photocatalytic activity.Ultraviolet light accounts for the energy of sunshine less than 5%, and the ratio of visible ray accounts for 45% left side
It is right.So exploitation designs the visible light catalyst of efficient responding to visible light as research tendency in recent years.
Bismuth tungstate（Bi2WO6）It is a kind of visible light response catalyst to attract attention in recent years, its band-gap energy is about
2.69eV, 420-460nm visible ray can be responded, there is unique electronic structure, excellent visible absorption ability, be considered as
It is a kind of potential excellent visible light catalyst.The wolframic acid bismuth catalyst of nanostructured can effectively strengthen light because specific surface area improves
Catalytic performance, but the too small easily reunion of particle diameter simultaneously reduces catalytic performance, is unfavorable for it in addition and is separated from degradation solution, easily
Secondary pollution is caused to environment.Therefore from practical standpoint, it is necessary to bismuth tungstate is loaded into certain load using immobilization technology
It could be used on body.Activated carbon is a kind of porous solid carbonaceous of black, and its hole is flourishing, has huge specific surface area, has
Very strong absorption property, it is a kind of preferable carrier.The absorption property of activated carbon and bismuth tungstate photocatalytic activity are combined,
Non-selectivity completeness using activated carbon to the efficient absorption of pollutant and bismuth tungstate to contaminant degradation mineralising so that negative
Load type bismuth tungstate, but also with preferable sedimentation separation property, carries while catalytic activity is kept for the recycling of catalyst
For advantage.
The content of the invention
In order to solve the problems of the prior art, a kind of photocatalysis performance of the present invention is good, the support type that is easily isolated and recycled
Bismuth tungstate photocatalyst and a kind of simple and convenient, easily controllable, the cheap environmentally friendly supported bismuth tungstate photocatalyst of cost system
Preparation Method.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of activated carbon supported bismuth tungstate photocatalyst, the supported bismuth tungstate photocatalyst are by by bismuth tungstate and carrier
Granular activated carbon is compound and is formed, wherein：Bismuth tungstate is filled in the pore structure of carrier granular activated carbon.
Further, the particle diameter of the carrier granular activated carbon is 400-500 μm.
A kind of preparation method of activated carbon supported bismuth tungstate photocatalyst, comprises the following steps：
A. five water bismuth nitrates are dissolved with salpeter solution（Bi（NO3）3·5H2O）, and add disodium ethylene diamine tetraacetate
（Na2EDTA）, magnetic agitation formation system 1；
B. by tungstate dihydrate acid sodium（NaWO4·2H2O）It is dissolved in distilled water, and adds disodium ethylene diamine tetraacetate（Na2EDTA）, stir
Mix dissolving and form system 2；
C. system 2 is added dropwise in system 1 with syringe and forms mixed solution, after then adding 5-10g activation thereto
Activated carbon, stirred in constant temperature blender with magnetic force, adjust pH value of solution=3；
D. solution step c added after activated carbon is stirred to thick in 80 DEG C of waters bath with thermostatic control, then at 120 DEG C, vacuum
Dry 0.5-1h；
E. the dried products of step d are calcined 1-2h in 500 DEG C and obtain supported bismuth tungstate photocatalyst.
Further, in the step a, salpeter solution volume is 30-60ml；Five water bismuth nitrates（Bi（NO3）3·5H2O）
For 4-10g；Disodium ethylene diamine tetraacetate（Na2EDTA）For 1-3g；
Further, in the step b, distilled water volume 20-40ml；Tungstate dihydrate acid sodium（NaWO4·2H2O）For 1.5-4g；
Disodium ethylene diamine tetraacetate（Na2EDTA）For 0.5-1.5g.
Further, in the step a, the concentration of salpeter solution is 1mol/L.
Further, in the step c, the temperature of constant temperature blender with magnetic force stirring is 40-60 DEG C, mixing speed 1000r/
Min-1500r/min, mixing time 15-30min.
Further, in the step c, regulation pH value of solution uses NaOH solution of the concentration for 1mol/L.
Further, in the step c, the method for activated carbon activation is：The activated carbon after sieving is taken, is cleaned by ultrasonic and removes
The dust of activated carbon surface, then with salt acid soak 5h, neutrality is washed to, 100 DEG C are dried for standby.
Further, in the step c, the activated carbon after sieving is 20-40 mesh；
Further, the concentration of hydrochloric acid is 0.1mol/L.
A kind of activated carbon supported bismuth tungstate photocatalyst is in rhodamine B degradation dyestuff, o-nitrophenol and Microcystin
Application.
Compared with prior art, the invention has the advantages that：
The loose structure of activated carbon and strong adsorptivity have in the load of wolframic acid bismuth catalyst in the present invention, while can strengthen photocatalysis
Activity；Separation process is more prone to effective；The inventive method is simple, cost is low, easy to control.
Brief description of the drawings
Fig. 1 is the XRD of supported bismuth tungstate photocatalyst in the present invention；
Fig. 2 is the SEM figures of supported bismuth tungstate photocatalyst in the present invention；
Fig. 3 is that the photocatalysis performance of wolframic acid bismuth catalyst and supported bismuth tungstate catalyst in the present invention in the prior art compares
Figure.
Embodiment
The present invention is further described with reference to embodiment.
Embodiment 1
A kind of activated carbon supported bismuth tungstate photocatalyst, the supported bismuth tungstate photocatalyst are by by bismuth tungstate and carrier
Granular activated carbon is compound and is formed, wherein：Bismuth tungstate is filled in the pore structure of carrier granular activated carbon；The carrier granular is lived
Property charcoal particle diameter be 400-500 μm.
A kind of preparation method of activated carbon supported bismuth tungstate photocatalyst, weighs 4g Bi（NO3）3·5H2O is dissolved in 30ml nitre
Acid（The concentration of salpeter solution is 1mol/L）In, add 1g Na2EDTA, magnetic agitation 15min form solution A；Weigh 1.5g
NaWO4·2H2O is dissolved in 20ml distilled water, adds 0.5g Na2EDTA, stirring and dissolving form solution B, and solution B is injected
Solution A is added dropwise in device, then adds 5g activated carbons（Activated carbon activation method be：Take the activated carbon of 60 mesh after sieving, ultrasound
Cleaning removes the dust of activated carbon surface, then with salt acid soak 5h, is washed to neutrality, 100 DEG C are dried for standby）, in 50 DEG C of constant temperature
Magnetic agitation 15min on magnetic stirring apparatus, mixing speed 1500r/min, it is 1mol/L NaOH solutions regulation pH=3 with concentration,
Stirring in 80 DEG C of thermostat water baths is put into, to sticky shape, to be subsequently placed in 120 DEG C of vacuum drying chambers and dry 0.5h, by dried sample
Product are placed in 500 DEG C of roasting 1h in Muffle furnace and obtain supported bismuth tungstate photocatalyst.
A kind of activated carbon supported bismuth tungstate photocatalyst is in rhodamine B degradation dyestuff, o-nitrophenol and Microcystin
Application.
Embodiment 2
A kind of activated carbon supported bismuth tungstate photocatalyst, the supported bismuth tungstate photocatalyst are by by bismuth tungstate and carrier
Granular activated carbon is compound and is formed, wherein：Bismuth tungstate is filled in the pore structure of carrier granular activated carbon；The carrier granular is lived
Property charcoal particle diameter be 400-500 μm.
A kind of preparation method of activated carbon supported bismuth tungstate photocatalyst, weighs 10g Bi（NO3）3·5H2O is dissolved in 60ml
Nitric acid（1mol/L）In, add 3g Na2EDTA, magnetic agitation 30min form solution A；Weigh 4g NaWO4·2H2O is dissolved in
In 40ml distilled water, 1.5g Na are added2EDTA, stirring and dissolving form solution B, solution B are added dropwise using syringe molten
Liquid A, then add 10g activated carbons（Activated carbon activation method be：The activated carbon of 80 mesh after sieving is taken, is cleaned by ultrasonic except deactivation
The dust of property carbon surface, then with salt acid soak 5h, neutrality is washed to, 100 DEG C are dried for standby）, in 40 DEG C of constant temperature blender with magnetic force
Upper magnetic agitation 30min, mixing speed 1300r/min, pH=3 are adjusted with 1mol/L NaOH solutions, are put into 80 DEG C of waters bath with thermostatic control
Stirring is subsequently placed in 120 DEG C of vacuum drying chambers and dries 1h, dried sample is placed in 500 in Muffle furnace to sticky shape in pot
DEG C roasting 2h obtain supported bismuth tungstate photocatalyst.
A kind of activated carbon supported bismuth tungstate photocatalyst is in rhodamine B degradation dyestuff, o-nitrophenol and Microcystin
Application.
Embodiment 3
A kind of activated carbon supported bismuth tungstate photocatalyst, the supported bismuth tungstate photocatalyst are by by bismuth tungstate and carrier
Granular activated carbon is compound and is formed, wherein：Bismuth tungstate is filled in the pore structure of carrier granular activated carbon；The carrier granular is lived
Property charcoal particle diameter be 400-500 μm.
A kind of preparation method of activated carbon supported bismuth tungstate photocatalyst, weighs 7g Bi（NO3）3·5H2O is dissolved in 45ml nitre
Acid（1mol/L）In, add 2g Na2EDTA, magnetic agitation 30min form solution A；Weigh 2.75g NaWO4·2H2O is dissolved in
In 30ml distilled water, 1g Na are added2EDTA, stirring and dissolving form solution B, solution B are added dropwise into solution using syringe
A, then add 7.5g activated carbons（Activated carbon activation method be：The activated carbon of 40 mesh after sieving is taken, ultrasonic cleaning removes deactivation
The dust of carbon surface, then with salt acid soak 5h, neutrality is washed to, 100 DEG C are dried for standby）, in 60 DEG C of constant temperature blender with magnetic force
Magnetic agitation 20min, mixing speed 1000r/min, pH=3 are adjusted with 1mol/L NaOH solutions, are put into 80 DEG C of thermostat water baths
Middle stirring is subsequently placed in 120 DEG C of vacuum drying chambers and dries 0.75h, dried sample is placed in 500 in Muffle furnace to sticky shape
DEG C roasting 1.5h obtain supported bismuth tungstate photocatalyst.
A kind of activated carbon supported bismuth tungstate photocatalyst is in rhodamine B degradation dyestuff, o-nitrophenol and Microcystin
Application.
Photocatalysis performance is tested：Bi2WO6The performance test of/AC photochemical catalysts is completed in a double-jacket beaker.Drop
Solution liquid is the MC-LR solution that concentration is 2mg/L, and light source is 500 xenon lamps and is equipped with 420nm optical filter.In test experiments, take
5ml MC-LR solution adds 0.5gBi in test tube2WO6/ AC photochemical catalysts, are placed in chuck beaker.Before illumination, this is suspended
Liquid magnetic agitation at least 30min in the dark, to reach adsorption-desorption balance.In catalytic process, an examination is taken out every 10min
Pipe, centrifuge and remove photocatalyst granular, the concentration of MC-LR in supernatant is detected with high performance liquid chromatograph.
Fig. 3 is in pH=6.5, it is seen that sterling bismuth tungstate and supported bismuth tungstate photocatalyst 60min of the present invention under optical condition
The interior degraded situation to Microcystin.MC-LR concentration when wherein C0 is 0min, C are that the MC-LR detected in catalytic process is dense
Degree.As seen from the figure, in 60min, MC-LR is gradually degraded by catalyst, and supported bismuth tungstate catalyst is than pure bismuth tungstate
Degradation rate is bigger, and both are respectively 61%, 49%, illustrates the supported bismuth tungstate photocatalyst of the present invention and has than sterling bismuth tungstate
More preferable photocatalytic activity, there is more preferable degradation property to MC-LR.
Described above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
- A kind of 1. activated carbon supported bismuth tungstate photocatalyst, it is characterised in that：The supported bismuth tungstate photocatalyst is to pass through Bismuth tungstate and carrier granular activated carbon is compound and formed, wherein：Bismuth tungstate is filled in the pore structure of carrier granular activated carbon.
- 2. activated carbon supported bismuth tungstate photocatalyst according to claim 1, it is characterised in that：The carrier granular activity The particle diameter of charcoal is 400-500 μm.
- 3. the preparation method of activated carbon supported bismuth tungstate photocatalyst according to claim 1 or 2, it is characterised in that bag Include following steps：A. five water bismuth nitrates are dissolved with salpeter solution, and adds disodium ethylene diamine tetraacetate, magnetic agitation forms system 1；B. tungstate dihydrate acid sodium is dissolved in distilled water, and adds disodium ethylene diamine tetraacetate, stirring and dissolving forms system 2；C. system 2 is added dropwise in system 1 and forms mixed solution, the activated carbon then added thereto after 5-10g activation, Stirred in constant temperature blender with magnetic force, adjust pH value of solution=3；D. solution step c added after activated carbon is stirred to thick in 80 DEG C of waters bath with thermostatic control, then at 120 DEG C, vacuum Dry 0.5-1h；E. the dried products of step d are calcined 1-2h in 500 DEG C and obtain supported bismuth tungstate photocatalyst.
- 4. the preparation method of activated carbon supported bismuth tungstate photocatalyst according to claim 3, it is characterised in that：The step In rapid a, salpeter solution volume is 30-60ml；Five water bismuth nitrates are 4-10g；Disodium ethylene diamine tetraacetate is 1-3g；The step In b, distilled water volume 20-40ml；Tungstate dihydrate acid sodium is 1.5-4g；Disodium ethylene diamine tetraacetate is 0.5-1.5g.
- 5. the preparation method of activated carbon supported bismuth tungstate photocatalyst according to claim 3, it is characterised in that：The step In rapid a, the concentration of salpeter solution is 1mol/L.
- 6. the preparation method of activated carbon supported bismuth tungstate photocatalyst according to claim 3, it is characterised in that：The step In rapid c, the temperature of constant temperature blender with magnetic force stirring is 40-60 DEG C, mixing speed 1000r/min-1500r/min, mixing time For 15-30min.
- 7. the preparation method of activated carbon supported bismuth tungstate photocatalyst according to claim 3, it is characterised in that：The step In rapid c, regulation pH value of solution uses NaOH solution of the concentration for 1mol/L.
- 8. the preparation method of activated carbon supported bismuth tungstate photocatalyst according to claim 3, it is characterised in that：The step In rapid c, the method for activated carbon activation is：The activated carbon after sieving is taken, is cleaned by ultrasonic the dust for removing activated carbon surface, then use salt Acid soak 5h, neutrality is washed to, 100 DEG C are dried for standby.
- 9. the preparation method of activated carbon supported bismuth tungstate photocatalyst according to claim 8, it is characterised in that：The step In rapid c, the activated carbon after sieving is 20-40 mesh；The concentration of hydrochloric acid is 0.1mol/L.
- 10. activated carbon supported bismuth tungstate photocatalyst according to claim 1 or 2 is in rhodamine B degradation dyestuff, adjacent nitro The application of phenol and Microcystin.
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| CN111036273A (en) * | 2019-12-30 | 2020-04-21 | 吉林农业大学 | Corn straw biochar and Bi for efficiently degrading organic pollutants2WO6Method for preparing photocatalyst |
| CN111573673A (en) * | 2020-05-19 | 2020-08-25 | 南京信息工程大学 | Preparation method and application of sulfonated activated carbon |
| CN113788504A (en) * | 2021-09-30 | 2021-12-14 | 中国矿业大学 | Bismuth tungstate-based photocatalytic reactor and mineral processing wastewater degradation system |
| CN114345380A (en) * | 2022-01-18 | 2022-04-15 | 西南交通大学 | Bismuth oxychloride/bismuth tungstate nano-catalyst and preparation method and application thereof |
| CN115368911A (en) * | 2022-09-02 | 2022-11-22 | 东莞理工学院 | Method for restoring soil polluted by fluoroquinolone antibiotics |
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