CN101757908A - Method for preparing Bi2WO6 with high efficiency and visible light photocatalytic activity by adjusting pH - Google Patents
Method for preparing Bi2WO6 with high efficiency and visible light photocatalytic activity by adjusting pH Download PDFInfo
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- CN101757908A CN101757908A CN200910245148A CN200910245148A CN101757908A CN 101757908 A CN101757908 A CN 101757908A CN 200910245148 A CN200910245148 A CN 200910245148A CN 200910245148 A CN200910245148 A CN 200910245148A CN 101757908 A CN101757908 A CN 101757908A
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Abstract
The invention discloses a method for preparing Bi2WO6 with high efficiency and visible light photocatalytic activity by adjusting the pH, which belongs to the fields of catalyst preparation and environment pollution control. The method comprises the following steps: respectively dissolving Bi(NO3)3.5H2O into HNO3solution and dissolving Na2WO4.2H2O into NaOH solution to prepare solution; transferring and taking two kinds of solutions for fully mixing to obtain a precursor of Bi2WO6; stirring the mixed solution, ultrasound homogenizing and adjusting the pH value of the mixed solution with HNO3 and NaOH dilute solution; placing the adjusted solution into a reaction kettle for hydrothermal reaction; and cooling, centrifuging and drying the reactive product. In the invention, a Bi2WO6 photocatalyst with high photocatalytic activity can be prepared by using a hydrothemal method and adjusting different pH values. Under the radiation of visible light, the photocatalytic effect for degrading the activity of brilliant red X-3B is far better than that of P-25 TiO2; and under the sunlight irradiation, the photocatalytic effect is better than that of the P-25 TiO2. Under the condition of simulating the sunlight, the invention has good effect of removing an internal division chaff interferent bisphenol A.
Description
Technical field
The invention belongs to Preparation of Catalyst and environmental pollution improvement field, particularly a kind of method with photochemical catalyst of high catalytic activity.
Background technology
Nanometer technology has been subjected to paying close attention to widely as a kind of water technology that has potentiality.Nano-photo catalytic oxidation technology multiple organic pollution in the degradation water more efficiently wherein, and have characteristics such as degradation speed is fast, applied range.
TiO
2, advantages such as chemical stability good, oxidability strong, non-secondary pollution nontoxic with it become desirable catalyst, TiO
2In degradation water difficult remove organic pollution aspect a large amount of research has been arranged.But TiO
2Energy gap is 3.2ev, and only absorbent wavelength is less than the ultraviolet light of 387nm, and this part ultraviolet light only accounts for 4%-6% in solar spectrum, and the sunshine utilization rate is low.
Improve the utilization rate of catalyst, mainly set about from two aspects to sunshine: the one, to TiO
2Carry out modification; The 2nd, research novel visible catalysis material.TiO
2Though modification make photochemical catalyst that certain response arranged in the visual field, this is often to sacrifice TiO
2The ultraviolet light activity be cost, seek cheapness, environmental friendliness and have the trend that high performance visible-light photocatalysis material will be photocatalysis technology research.
Recently, scientists has been found a series of tungstates photochemical catalysts with photoresponse, as bismuth tungstate, and Zinc Tungstate, wolframic acid silver etc.Semi-conducting materials such as tungstates because of its its specific structure and physicochemical properties, are subject to people's attention day by day, study very active.Systematically study the relation between relation, pattern and the photocatalysis of the characteristics of luminescence of semiconductor material system such as tungstates and crystal structure, can be designing and developing of advanced luminescent material and catalysis material theoretical foundation is provided.Studies show that Bi
2WO
6Under radiation of visible light, can be from AgNO
3Decomposition water obtains O in the solution
2, and the CHCl that can degrade
3And CH
3Pollutants such as CHO.
The semi-conductive valence band of tungstates is formed by the outermost layer 6s and the O2p orbital hybridization of metallic atom, has higher oxidation activity and charge mobility; Be different from the titanium dioxide of doping, the tungstates photochemical catalyst has at visible region more precipitous can be with ABSORPTION EDGE, show that their visible absorption results from the band-to-band transition of itself, but not the effect of impurity energy level, avoided the formed complex centre of impurity effectively and reduce catalytic efficiency.The tungstates photochemical catalyst contains WO simultaneously
6Mostly have unique layer structure, catalytic reaction is mainly carried out in interlayer space, play " two dimension " photocatalysis.Yet the researcher adopts solid phase method synthetic mostly, and the catalyst granules particle diameter that is obtained by this method is bigger, and specific area is little, and pollutant is less in the absorption of catalyst surface, and photocatalytic activity is not very high.
Summary of the invention
The present invention is in conjunction with existing bismuth tungstate technology of preparing, through conditional filtering, prepares that a kind of particle diameter is little, degree of crystallinity is high, the high Bi of catalytic activity under the sunshine
2WO
6
Technical scheme of the present invention:
Prepare high efficiency and visible light photocatalytic activity Bi by regulating pH
2WO
6Method, concrete steps are as follows:
1) with Bi (NO
3)
35H
2O is dissolved in HNO
3In the solution, wiring solution-forming;
2) with Na
2WO
42H
2O is dissolved in the NaOH solution, wiring solution-forming;
3) removing step 1) solution that makes is in beaker, under strong magnetic agitation, with step 2) solution that makes dropwise joins in the aforementioned beaker, fully mixes; Obtain the precursor of prepared catalyst;
4) mixed liquor is stirred, ultrasonic homogenizing is used HNO
3Regulate the pH value with the NaOH weak solution, the solution that mixes up pH is put in carries out hydro-thermal reaction in the reactor;
5) after hydro-thermal reaction is finished, naturally cool to room temperature, centrifugal, oven dry promptly obtains the photochemical catalyst of high catalytic activity under the sunshine, grinds standby.
Bi (NO in the described step 1)
3)
35H
2The solution concentration of O is 0.025-0.1mol/L.
Described step 2) Na in
2WO
42H
2The solution concentration of O is 0.025-0.1mol/L.
PH in the described step 4) is respectively 1-13.
Reactor is the stainless steel cauldron with polytetrafluoroethylliner liner in the described step 4).
Hydrothermal temperature is 140 ℃ in the described step 4), reaction time 20h.
Centrifugal with distilled water and absolute ethyl alcohol in the described step 5), bake out temperature is 120 ℃, 4h.
Grinding used utensil in the described step 5) is agate mortar.
The present invention's hydro-thermal method by regulating different pH, is prepared high efficiency and visible light photocatalytic activity Bi
2WO
6Catalyst.The effect of photocatalytic degradation reactive brilliant red x-3b is much larger than P-25TiO under the visible radiation
2, under the solar light irradiation, the photocatalysis effect also is better than P-25TiO
2Under the condition of simulated solar irradiation, internally divide the chaff interference bisphenol-A that good effect of removing is arranged.
Description of drawings
Fig. 1 is the Bi of embodiment 1 preparation
2WO
6The XRD figure spectrum of photochemical catalyst
Fig. 2 is the Bi of embodiment 1 preparation
2WO
6The SEM of photochemical catalyst, TEM shape appearance figure
Fig. 3 is the Bi of embodiment 1 preparation
2WO
6The UV-Vis curve of photochemical catalyst
Fig. 4 is the Bi of embodiment 1 preparation
2WO
6The removal effect of photochemical catalyst degraded reactive brilliant red x-3b under visible light and direct solar light irradiation
Fig. 5 is the Bi of embodiment 2 preparations
2WO
6Under visible light, the degrade removal effect of reactive brilliant red x-3b of photochemical catalyst
Fig. 6 is the Bi of preparation among the embodiment one
2WO
6Under simulated solar irradiation, the degrade effect of incretion interferent BPA of photochemical catalyst
The specific embodiment
Embodiment 1:
Prepare high efficiency and visible light photocatalytic activity Bi by regulating pH
2WO
6Concrete processing step as follows:
1) takes by weighing 48.51g Bi (NO
3)
35H
2O is dissolved in 1mol/L HNO
3In the solution, be made into the Bi (NO of 1000mL0.1mol/L
3)
35H
2O solution;
2) take by weighing the Na of 16.49g
2WO
42H
2O is dissolved in the 1mol/L NaOH solution, is made into the Na of 1000mL0.05mol/L
2WO
42H
2O solution;
3) pipette the Bi (NO of 20mL 0.1mol/L
3)
35H
2O solution is in the 50mL beaker, under strong magnetic agitation, with the Na of 20mL0.05mol/L
2WO
42H
2O solution dropwise joins in the small beaker, with Bi (NO
3)
35H
2O fully mixes, and the mixed liquor that obtains is the precursor of prepared catalyst;
4) with the strong magnetic agitation 10min of mixed liquor, ultrasonic homogenizing 30min uses HNO
3Regulate the pH value with the weak solution of NaOH, to pH11, the solution that mixes up pH is put in 50mL has in the stainless steel cauldron of polytetrafluoroethylliner liner, hydrothermal reaction condition is 140 ℃, 20h.
5) after hydro-thermal reaction is finished, naturally cool to room temperature, use distilled water and absolute ethyl alcohol centrifugal respectively, in 120 ℃ of baking ovens, dry.Promptly obtain the photochemical catalyst of high catalytic activity under the sunshine.
By the XRD material phase analysis, prepared catalyst is the Bi of JCPDS 39-0526
2WO
6By SEM, tem analysis, prepared catalyst is the laminar nano thin slice.Analyze prepared Bi by UV-vis DRS
2WO
6Catalyst can have response with light to the 450nm place.
Embodiment 2:
Prepare highlight catalytic active Bi by regulating pH
2WO
6Concrete processing step as follows:
1) takes by weighing 48.51g Bi (NO
3)
35H
2O is dissolved in the 1mol/L HNO3 solution, is made into the Bi (NO of 1000mL0.1mol/L
3)
35H
2O solution;
2) take by weighing the Na of 8.25g
2WO
42H
2O is dissolved in the 1mol/L NaOH solution, is made into the Na of 1000mL0.025mol/L
2WO
42H
2O solution;
3) pipette the Bi (NO of 20mL 0.1mol/L
3)
35H
2O solution is in the 50mL beaker, under strong magnetic agitation, with the Na of 20mL0.05mol/L
2WO
42H
2O solution dropwise joins in the small beaker, with Bi (NO
3)
35H
2O fully mixes, and the mixed liquor that obtains is the precursor of prepared catalyst;
4) with the strong magnetic agitation 10min of mixed liquor, ultrasonic homogenizing 30min uses HNO
3Regulate the pH value with the weak solution of NaOH, to pH1, the solution that mixes up pH is put in 50mL has in the stainless steel cauldron of polytetrafluoroethylliner liner, hydrothermal reaction condition is 140 ℃, 20h.
5) after hydro-thermal reaction is finished, naturally cool to room temperature, use distilled water and absolute ethyl alcohol centrifugal respectively, in 120 ℃ of baking ovens, dry.Promptly obtain the photochemical catalyst of high catalytic activity under the sunshine.
Characterize by XRD, SEM, TEM, prepared catalyst is the Bi of JCPDS 39-0526
2WO
6, catalyst is the laminar nano thin slice.Analyze prepared Bi by UV-vis DRS
2WO
6Catalyst can have response with light to the 450nm place.
Embodiment 3:
Accurately measure the reactive brilliant red x-3b dyestuff 50mL of 20ppm, place the 50mL quartz test tube, take by weighing the Bi of preparation among the embodiment 1
2WO
6Catalyst 0.1g under the magnetic agitation of 300rpm, uses the 800W xenon lamp radiation in test tube, add the filter plate of 400nm.Get 6mL solution behind the 60min and cross 0.45 μ m filter membrane, it is the cuvette of 1cm that filtrate is placed light path, measures absorbance with spectrophotometer under the 538nm wavelength.Obtain the surplus ratio of reactive brilliant red x-3b according to calibration curve, thus the clearance of calculated activity bright red X-3B.Bi under the radiation of visible light
2WO
6Clearance to reactive brilliant red x-3b in 60min is 92.15%, is about P-25TiO
210 times.
Embodiment 4:
Accurately measure the reactive brilliant red x-3b dyestuff 50mL of 20ppm, place the 100mL small beaker, take by weighing the Bi of preparation among the embodiment 1
2WO
6Catalyst 0.1g under the magnetic agitation of 300rpm, is positioned under the sunshine in beaker, directly radiation.Get 6mL solution behind the 60min and cross 0.45 μ m filter membrane, it is the cuvette of 1cm that filtrate is placed light path, measures absorbance with spectrophotometer under the 538nm wavelength.Obtain the surplus ratio of reactive brilliant red x-3b according to calibration curve, thus the clearance of calculated activity bright red X-3B.Under the direct solar light irradiation, Bi
2WO
6Clearance to reactive brilliant red x-3b is 70.05%, greater than P-25TiO
2Clearance to reactive brilliant red x-3b.
Embodiment 5
Accurately measure the reactive brilliant red x-3b dyestuff 50mL of 20ppm, place the 50mL quartz test tube, take by weighing the Bi of preparation among the embodiment 2
2WO
6Catalyst 0.1g under the magnetic agitation of 300rpm, uses the 800W xenon lamp radiation in test tube, add the filter plate of 400nm.Get 6mL solution behind the 60min and cross 0.45 μ m filter membrane, it is the cuvette of 1cm that filtrate is placed light path, measures absorbance with spectrophotometer under the 538nm wavelength.Obtain the surplus ratio of reactive brilliant red x-3b according to calibration curve, thus the clearance of calculated activity bright red X-3B.Bi under the radiation of visible light
2WO
6Clearance to reactive brilliant red x-3b in 60min is 84.06%, is about P-25TiO
29 times.
Accurately measure the incretion interferent bisphenol-A 250mL of 20ppm, place the 250mL circular reactor, take by weighing the Bi of preparation among the embodiment 1
2WO
6Catalyst 0.25g is in test tube, and lucifuge stirs 30min, and with 800W xenon lamp simulated solar light radiation 60min, 0.45 μ m filter membrane is crossed in sampling at regular intervals, detects by high performance liquid chromatography.Obtain the surplus ratio of bisphenol-A according to calibration curve, thereby calculate the clearance of bisphenol-A.Use P-25TiO simultaneously
2Do check experiment.The simulated solar irradiation irradiation is Bi down
2WO
6Nearly 100% to the clearance of bisphenol-A in 60min, and P-25 TiO
2To the clearance of bisphenol-A less than 30%.
Claims (8)
1. one kind prepares high efficiency and visible light photocatalytic activity Bi by regulating pH
2WO
6Method, it is characterized in that concrete steps are as follows:
1) with Bi (NO
3)
35H
2O is dissolved in HNO
3In the solution, wiring solution-forming;
2) with Na
2WO
42H
2O is dissolved in the NaOH solution, wiring solution-forming;
3) removing step 1) solution that makes is in beaker, under strong magnetic agitation, with step 2) solution that makes dropwise joins in the aforementioned beaker, fully mixes;
4) with the mixed liquor magnetic agitation, ultrasonic homogenizing is used HNO
3Regulate the pH value with the NaOH weak solution, the solution that mixes up pH is put in carries out hydro-thermal reaction in the reactor;
5) after hydro-thermal reaction is finished, naturally cool to room temperature, centrifugal, oven dry.
2. according to claim 1ly prepare high efficiency and visible light photocatalytic activity Bi by regulating pH
2WO
6Method, it is characterized in that: Bi (NO in the described step 1)
3)
35H
2The solution concentration of O is 0.025-0.1mol/L.
3. according to claim 1ly prepare high efficiency and visible light photocatalytic activity Bi by regulating pH
2WO
6Method, it is characterized in that: described step 2) in Na
2WO
42H
2The solution concentration of O is 0.025-0.1mol/L.
4. according to claim 1ly prepare high efficiency and visible light photocatalytic activity Bi by regulating pH
2WO
6Method, it is characterized in that: the pH in the described step 4) is 1-13.
5. according to claim 1ly prepare high efficiency and visible light photocatalytic activity Bi by regulating pH
2WO
6Method, it is characterized in that: reactor is the stainless steel cauldron with polytetrafluoroethylliner liner in the described step 4).
6. according to claim 1ly prepare high efficiency and visible light photocatalytic activity Bi by regulating pH
2WO
6Method, it is characterized in that: hydrothermal temperature is 140 ℃ in the described step 4), the reaction time is 20h.
7. according to claim 1ly prepare high efficiency and visible light photocatalytic activity Bi by regulating pH
2WO
6Method, it is characterized in that: centrifugal with distilled water and absolute ethyl alcohol in the described step 5), bake out temperature is 120 ℃, and the time is 4h.
8. according to claim 1ly prepare high efficiency and visible light photocatalytic activity Bi by regulating pH
2WO
6Method, it is characterized in that: grinding used utensil in the described step 5) is agate mortar.
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|---|---|---|---|
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|---|---|---|---|
| CN200910245148A CN101757908A (en) | 2009-12-29 | 2009-12-29 | Method for preparing Bi2WO6 with high efficiency and visible light photocatalytic activity by adjusting pH |
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|---|---|
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ID=42489387
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| CN102553570A (en) * | 2011-12-20 | 2012-07-11 | 陕西科技大学 | Microwave hydrothermal preparation method for BiO2 and bismuth tungstate composite semiconductor |
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| CN102674461A (en) * | 2012-05-15 | 2012-09-19 | 陕西科技大学 | Preparation method of laminar-card-structure bisumth tungstate microcrystals |
| CN103191725A (en) * | 2013-04-26 | 2013-07-10 | 南京信息工程大学 | BiVO4/Bi2WO6 composite semiconductor material as well as hydrothermal preparation method and application thereof |
| CN103521237A (en) * | 2013-11-01 | 2014-01-22 | 南昌航空大学 | Method for preparing Fe3O4/SiO2/Bi2WO6 magnetic microsphere photocatalyst |
| CN103611526A (en) * | 2013-03-02 | 2014-03-05 | 西北大学 | Preparation method for bismuth tungstate microsphere with core-shell structure |
| CN106390992A (en) * | 2016-11-08 | 2017-02-15 | 广西大学 | Preparation method and photocatalytic performance of Bi2WO6-x micro-nano material |
| CN107020081A (en) * | 2017-04-18 | 2017-08-08 | 浙江大学 | A kind of visible light catalytic coating using concrete as matrix and preparation method thereof |
| CN108543531A (en) * | 2018-05-04 | 2018-09-18 | 南开大学 | Three-dimensional meso-hole Bi2WO6Nanosphere and its preparation method and application |
| CN110373891A (en) * | 2019-07-16 | 2019-10-25 | 东华大学 | Load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene and preparation method thereof |
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2009
- 2009-12-29 CN CN200910245148A patent/CN101757908A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102553570A (en) * | 2011-12-20 | 2012-07-11 | 陕西科技大学 | Microwave hydrothermal preparation method for BiO2 and bismuth tungstate composite semiconductor |
| CN102553570B (en) * | 2011-12-20 | 2014-06-04 | 陕西科技大学 | Microwave hydrothermal preparation method for BiO2 and bismuth tungstate composite semiconductor |
| CN102600857A (en) * | 2012-03-01 | 2012-07-25 | 浙江大学 | Preparation method of carbon ball-loaded CuO-BiVO4 heterojunction compound photocatalyst |
| CN102674461A (en) * | 2012-05-15 | 2012-09-19 | 陕西科技大学 | Preparation method of laminar-card-structure bisumth tungstate microcrystals |
| CN103611526A (en) * | 2013-03-02 | 2014-03-05 | 西北大学 | Preparation method for bismuth tungstate microsphere with core-shell structure |
| CN103191725A (en) * | 2013-04-26 | 2013-07-10 | 南京信息工程大学 | BiVO4/Bi2WO6 composite semiconductor material as well as hydrothermal preparation method and application thereof |
| CN103521237A (en) * | 2013-11-01 | 2014-01-22 | 南昌航空大学 | Method for preparing Fe3O4/SiO2/Bi2WO6 magnetic microsphere photocatalyst |
| CN106390992A (en) * | 2016-11-08 | 2017-02-15 | 广西大学 | Preparation method and photocatalytic performance of Bi2WO6-x micro-nano material |
| CN107020081A (en) * | 2017-04-18 | 2017-08-08 | 浙江大学 | A kind of visible light catalytic coating using concrete as matrix and preparation method thereof |
| CN107020081B (en) * | 2017-04-18 | 2020-05-12 | 浙江大学 | Visible light catalytic coating with concrete as matrix and preparation method thereof |
| CN108543531A (en) * | 2018-05-04 | 2018-09-18 | 南开大学 | Three-dimensional meso-hole Bi2WO6Nanosphere and its preparation method and application |
| CN110373891A (en) * | 2019-07-16 | 2019-10-25 | 东华大学 | Load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene and preparation method thereof |
| CN111268758A (en) * | 2020-03-04 | 2020-06-12 | 安徽晋煤中能化工股份有限公司 | Treatment method of phenol wastewater |
| CN112156803A (en) * | 2020-09-28 | 2021-01-01 | 东北大学 | Photocatalytic composite material and preparation method and application thereof |
| CN112156803B (en) * | 2020-09-28 | 2021-09-10 | 东北大学 | Photocatalytic composite material and preparation method and application thereof |
| CN113713802A (en) * | 2021-09-15 | 2021-11-30 | 辽宁大学 | CoWO (cobalt oxide tungsten trioxide)4/Bi2WO6Composite acoustic catalyst and preparation method and application thereof |
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Application publication date: 20100630 |