CN107308957A - A kind of spherical Bi2S3/Bi2WO6The preparation method of heterojunction photocatalysis material - Google Patents
A kind of spherical Bi2S3/Bi2WO6The preparation method of heterojunction photocatalysis material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 45
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 38
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 4
- 239000012798 spherical particle Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- -1 polyethylene Polymers 0.000 claims description 4
- WPZFLQRLSGVIAA-UHFFFAOYSA-N sodium tungstate dihydrate Chemical compound O.O.[Na+].[Na+].[O-][W]([O-])(=O)=O WPZFLQRLSGVIAA-UHFFFAOYSA-N 0.000 claims description 4
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims description 2
- 150000004677 hydrates Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- 150000004040 pyrrolidinones Chemical class 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 11
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000005342 ion exchange Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 description 10
- 229960003405 ciprofloxacin Drugs 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000003708 ampul Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000004847 absorption spectroscopy Methods 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- PMNLUUOXGOOLSP-UHFFFAOYSA-N 2-mercaptopropanoic acid Chemical class CC(S)C(O)=O PMNLUUOXGOOLSP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 150000001243 acetic acids Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a kind of spherical Bi2S3/Bi2WO6The preparation method of heterojunction photocatalysis material, belongs to the synthesis technical field of catalysis material.Technical scheme main points are：A kind of spherical Bi2S3/Bi2WO6The preparation method of heterojunction photocatalysis material, specifically includes spherical Bi2WO6Preparation and spherical Bi2S3/Bi2WO6The steps such as the preparation of heterojunction photocatalysis material, the spherical Bi2S3/Bi2WO6Heterojunction photocatalysis material is by Bi2WO6Nanometer sheet and Bi2S3The particle diameter of nanometer rods composition is 35 μm of spherical particle.The present invention synthesizes spherical Bi using hydro-thermal method and ion-exchange2S3/Bi2WO6Heterojunction photocatalysis material, both are combined to the advantage for giving full play to two kinds of materials, shortcoming between making up, the separation in electronics and hole can be effectively facilitated, absorption region of the composite to light can be widened again, so as to improve the efficiency and catalytic efficiency of bismuth based semiconductor catalysis material, higher visible light catalytic performance is shown.
Description
Technical field
The invention belongs to the synthesis technical field of catalysis material, and in particular to a kind of spherical Bi2S3/Bi2WO6Hetero-junctions
The preparation method of catalysis material.
Background technology
With the development of the social economy, this three major issues of environment, material, the energy are increasingly protruded, photocatalysis technology has
Inexpensive, environment-friendly the features such as, so increasing scientific research personnel is solved above-mentioned this using photocatalysis technology and three asked greatly
Topic.Photocatalysis technology depends primarily on catalysis material, the photochemical catalyst of one pack system be difficult effectively and meanwhile using visible ray and
Ultraviolet light, and photo-generate electron-hole is combined probability height, limits its photocatalytic activity.
Bi2WO6Crystal structure it is fairly simple, be typical type n semiconductor material, it is by (Bi2O2)2+(WO6)2-
The oxide of the laminated perovskite structure alternately constituted, the space of interlayer can provide place for photocatalysis.And Bi2WO6Valency
Band current potential is 3.18eV, and conduction band is 0.54eV, and energy gap is about 2.64eV, shows that bismuth tungstate can only utilize a small amount of visible ray.
It is used as a kind of typical bismuthino multifunctional material, Bi2S3Band gap width between 1.2-1.7eV, under the irradiation of visible ray,
It is highly susceptible to excite and generates photo-generate electron-hole pair, but is easier to be combined, and it is unstable during the course of the reaction.
Bi2S3/Bi2WO6Heterojunction photocatalysis material makes full use of Bi2S3And Bi2WO6Cooperative effect, compensate for each other it
Between shortcoming, be both effectively promoted the separation in electronics and hole, and absorption region of the composite to light widened again, so as to improve
The efficiency and catalytic efficiency of bismuth based semiconductor catalysis material, but still not on synthesizing spherical Bi2S3/Bi2WO6Hetero-junctions
Catalysis material is to improve the relevant report of its photocatalysis performance.
The content of the invention
It is simple to operate and friendly to environment and with good visible light catalytic present invention solves the technical problem that there is provided one kind
The spherical Bi of activity2S3/Bi2WO6The preparation method of heterojunction photocatalysis material.
The present invention is to solve above-mentioned technical problem to adopt the following technical scheme that, a kind of spherical Bi2S3/Bi2WO6Hetero-junctions light
The preparation method of catalysis material, it is characterised in that concretely comprise the following steps：
（1）Spherical Bi2WO6Preparation, polyvinylpyrrolidone and five nitric hydrate bismuths are dissolved in ethanol, glacial acetic acid and deionization
In the mixed solution of water, it is stirred at room temperature after 15min and obtains solution A, takes Disodium tungstate (Na2WO4) dihydrate to be dissolved in deionized water and obtain molten
Liquid B, solution B under stirring be added in solution A and be well mixed, and mixed solution is transferred in reactor in 180
DEG C reaction 3h, be cooled to room temperature, by precipitation water and absolute ethyl alcohol cyclic washing, then obtain lamina stack in 60 DEG C of vacuum drying
Long-pending spherical Bi2WO6；
（2）Spherical Bi2S3/Bi2WO6The preparation of heterojunction photocatalysis material, by spherical Bi2WO6It is scattered in deionized water, then according to
Secondary addition mercaptopropionic acid and thioacetamide, wherein Bi2WO6Molar ratio with thioacetamide is 2:1, stirring mixing is equal
It is 10.5 to adjust the pH value of mixed solution with sodium hydroxide solution after even, be further continued for being transferred to after being uniformly mixed in reactor in
180 DEG C of reaction 3h, then centrifuge gained sediment, are washed with deionized water and absolute ethyl alcohol after 60 DEG C of vacuum drying
Spherical Bi is made2S3/Bi2WO6Heterojunction photocatalysis material, the spherical Bi2S3/Bi2WO6Heterojunction photocatalysis material be by
Bi2WO6Nanometer sheet and Bi2S3The particle diameter of nanometer rods composition is 3-5 μm of spherical particle.
Further preferably, step（1）Described in five nitric hydrate bismuths and Disodium tungstate (Na2WO4) dihydrate molar ratio be 2:1,
The volume ratio of the ethanol, glacial acetic acid and deionized water is 1:1:3, the charge ratio of the five nitric hydrates bismuth and ethanol is
1mmol:The charge ratio of 5mL, the polyvinylpyrrolidone and five nitric hydrate bismuths is 0.2g:1mmol.
The present invention synthesizes spherical Bi using hydro-thermal method and ion-exchange2S3/Bi2WO6Heterojunction photocatalysis material, Bi2WO6
Not high, the Bi to visible light catalytic performance2S3Have outstanding visible light-responded, but pure Bi2S3Electron-hole pair separation is difficult, for
The advantage and disadvantage of above two catalysis material, both are combined the advantage for giving full play to two kinds of materials, lacking between making up
Point, can effectively facilitate the separation in electronics and hole, and absorption region of the composite to light can be widened again, so as to improve bismuth system
The efficiency and catalytic efficiency of conductor photocatalysis material, show higher visible light catalytic performance.Building-up process work of the present invention
Skill is simple, environmental protection, is adapted to large-scale production, is expected to produce good social and economic benefit.
Brief description of the drawings
Fig. 1 is Bi made from the embodiment of the present invention 12S3/Bi2WO6The FESEM figures of heterojunction photocatalysis material；
Fig. 2 is Bi made from the embodiment of the present invention 12S3/Bi2WO6The UV-Vis DRS collection of illustrative plates of heterojunction photocatalysis material；
Fig. 3 is Bi made from the embodiment of the present invention 12S3/Bi2WO6The XRD spectrum of heterojunction photocatalysis material；
Fig. 4 is Bi made from the embodiment of the present invention 12S3/Bi2WO6Heterojunction photocatalysis material is degraded ring third under visible light illumination
Sha Xing ultraviolet-visible absorption spectroscopy change curve.
Embodiment
The above to the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
Weigh 0.2g polyvinylpyrrolidones（PVP）5mL ethanol, 5mL glacial acetic acids and 15mL are dissolved in the nitric hydrate bismuths of 1mmol five
In the mixed solution of deionized water, 15min is stirred at room temperature and obtains solution A, then takes 0.5mmol Disodium tungstate (Na2WO4) dihydrates to be dissolved in
Solution B is obtained in 10mL deionized waters, solution B is slowly added into solution A in the state of stirring, 30min is again stirring for
Ensure that reaction reagent is well mixed, finally pour into mixed solution in the reactor that liner is polytetrafluoroethylene (PTFE) in 180 DEG C of reactions
3h, is cooled to room temperature, and precipitation is washed for several times with deionized water and absolute ethyl alcohol, transfers to dry in 60 DEG C in vacuum drying chamber
Dry 10h obtains spherical Bi2WO6；Take the spherical Bi of the above-mentioned preparations of 0.5mmol2WO6It is scattered in deionized water, sequentially adds
0.008mL mercaptopropionic acids and 0.25mmol thioacetamides, the hydrogen-oxygen for being 0.02mol/L with molar concentration after being uniformly mixed
The pH value for changing sodium solution regulation mixed solution is 10.5, is further continued for being transferred to after being uniformly mixed in reactor in 180 DEG C of reactions
3h, then centrifuges gained sediment, is washed with deionized water and absolute ethyl alcohol and ball is made after 60 DEG C of vacuum drying
Shape Bi2S3/Bi2WO6Heterojunction photocatalysis material.
Fig. 1 is Bi made from the present embodiment2S3/Bi2WO6The FESEM figures of heterojunction photocatalysis material, as seen from the figure
Sample is in spherical, a diameter of 3-5 μm, the spherical Bi2S3/Bi2WO6Heterojunction photocatalysis material is by Bi2WO6Nanometer sheet and Bi2S3
The particle diameter of nanometer rods composition is 3-5 μm of spherical particle.
Fig. 2 is Bi made from the present embodiment2S3/Bi2WO6The UV-Vis DRS collection of illustrative plates of heterojunction photocatalysis material.
Fig. 3 is Bi made from the present embodiment2S3/Bi2WO6The XRD spectrum of heterojunction photocatalysis material, can from figure
Go out（103）、（200）、（202）、（220）、（303）、（102）、（109）、（307）Stronger diffraction maximum is occurred in that at crystal face,
With Bi2WO6Standard card（JCPDS 26-1044）It coincide, is tetragonal phase bismuth tungstate, the XRD of heterojunction photocatalysis material
Except corresponding to Bi in spectrum2WO6Diffraction maximum outside, 2 θ=15.741 °, 17.657 °, 22.471 °, 23.780 °, 25.040 °,
Fainter diffraction maximum is occurred in that at 31.920 °, 35.751 °, 39.223 °, 45.666 °, 51.610 °, these parameters and Bi2S3
（JCPDS 65-2435）Standard card is consistent, illustrates also there is Bi in product2S3Generation.Being analyzed more than to obtain, prepared
Product is Bi2S3/Bi2WO6Heterojunction photocatalysis material.
Embodiment 2
Photocatalytic degradation Ciprofloxacin：Using 500W xenon lamps as light source, the filter plate for being equipped with 420nm obtains visible ray, i.e. ripple
The long light less than 420nm can not pass through, and can be effectively prevented from ultraviolet light interference, be around the internal quartz cooling for being connected with cooling water
Trap.Experimentation is as follows：40mg samples are weighed with electronic balance, it is slowly poured into quartz ampoule, then is measured with graduated cylinder
40mL mass concentrations are 5mg/L ciprofloxacin solution, are poured into the quartz ampoule equipped with sample, then ultrasonic in ultrasonic wave
30min, enables sample to be uniformly distributed, and then quartz ampoule is fixed in light-catalyzed reaction instrument.Cooling water is first opened, then is opened
Bubbling machine, bubbling 15min reaches adsorption-desorption balance, is then turned on xenon lamp power supply, treats that light stability starts timing, often
15min takes a sample, and samples taken volume is about 4mL, and the solution of taking-up is centrifuged on centrifuge, supernatant liquor is fallen
Go out, accurately measure its absorbance, obtain the degraded situation to Ciprofloxacin, so as to evaluate the visible light catalytic performance of sample.
Fig. 4 is Bi made from embodiment 12S3/Bi2WO6Degrade under visible light illumination ring third of heterojunction photocatalysis material is husky
The ultraviolet-visible absorption spectroscopy change curve of star.As seen from the figure, with the extension of light-catalyzed reaction time, Ciprofloxacin exists
The intensity of maximum absorption band at 277nm gradually weakens, and shows Bi2S3/Bi2WO6Heterojunction photocatalysis material has to Ciprofloxacin
There is preferable visible light photocatalytic degradation activity.
Embodiment above describes general principle, principal character and the advantage of the present invention, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. a kind of spherical Bi2S3/Bi2WO6The preparation method of heterojunction photocatalysis material, it is characterised in that concretely comprise the following steps：
（1）Spherical Bi2WO6Preparation, polyvinylpyrrolidone and five nitric hydrate bismuths are dissolved in ethanol, glacial acetic acid and deionization
In the mixed solution of water, it is stirred at room temperature after 15min and obtains solution A, takes Disodium tungstate (Na2WO4) dihydrate to be dissolved in deionized water and obtain molten
Liquid B, solution B under stirring be added in solution A and be well mixed, and mixed solution is transferred in reactor in 180
DEG C reaction 3h, be cooled to room temperature, by precipitation water and absolute ethyl alcohol cyclic washing, then obtain lamina stack in 60 DEG C of vacuum drying
Long-pending spherical Bi2WO6；
（2）Spherical Bi2S3/Bi2WO6The preparation of heterojunction photocatalysis material, by spherical Bi2WO6It is scattered in deionized water, then according to
Secondary addition mercaptopropionic acid and thioacetamide, wherein Bi2WO6Molar ratio with thioacetamide is 2:1, stirring mixing is equal
It is 10.5 to adjust the pH value of mixed solution with sodium hydroxide solution after even, be further continued for being transferred to after being uniformly mixed in reactor in
180 DEG C of reaction 3h, then centrifuge gained sediment, are washed with deionized water and absolute ethyl alcohol after 60 DEG C of vacuum drying
Spherical Bi is made2S3/Bi2WO6Heterojunction photocatalysis material, the spherical Bi2S3/Bi2WO6Heterojunction photocatalysis material be by
Bi2WO6Nanometer sheet and Bi2S3The particle diameter of nanometer rods composition is 3-5 μm of spherical particle.
2. spherical Bi according to claim 12S3/Bi2WO6The preparation method of heterojunction photocatalysis material, it is characterised in that：
Step（1）Described in five nitric hydrate bismuths and Disodium tungstate (Na2WO4) dihydrate molar ratio be 2:1, the ethanol, glacial acetic acid and go
The volume ratio of ionized water is 1:1:3, the charge ratio of the five nitric hydrates bismuth and ethanol is 1mmol:5mL, the polyethylene
The charge ratio of pyrrolidones and five nitric hydrate bismuths is 0.2g:1mmol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710502025.5A CN107308957B (en) | 2017-06-27 | 2017-06-27 | Spherical Bi2S3/Bi2WO6Preparation method of heterojunction photocatalytic material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108355678A (en) * | 2018-03-09 | 2018-08-03 | 南昌航空大学 | A kind of compound micron bouquet of artificial gold-bismuth tungstate and its preparation method and application |
| CN108394956A (en) * | 2018-04-09 | 2018-08-14 | 沈阳化工大学 | A method of degradation antibiotic Ciprofloxacin Hydrochloride |
| CN108607498A (en) * | 2018-05-23 | 2018-10-02 | 四川理工学院 | A kind of preparation method and application of the enhanced bismuth tungstate of absorption property |
| CN108946863A (en) * | 2018-08-08 | 2018-12-07 | 辽宁大学 | A method of ultrasonotomography antibiotic waste water is catalyzed using copper tungstate |
| CN109046323A (en) * | 2018-10-18 | 2018-12-21 | 盐城工学院 | A kind of visible light catalyst CQDs/Bi2WO6And its preparation method and application |
| CN111167478A (en) * | 2020-01-08 | 2020-05-19 | 湖北大学 | CdS-Bi2WO6Application of semiconductor Z-type heterojunction in photocatalytic degradation of ethylene |
| CN111203239A (en) * | 2020-02-27 | 2020-05-29 | 齐鲁工业大学 | Bismuth tungstate/bismuth sulfide/molybdenum disulfide heterojunction ternary composite material and preparation method and application thereof |
| CN113235124A (en) * | 2021-05-18 | 2021-08-10 | 西北师范大学 | S-FeOOH/bismuth vanadate composite photo-anode and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105800687A (en) * | 2016-04-28 | 2016-07-27 | 江苏大学 | Method for preparing bismuth sulfide nanorod |
| CN106477629A (en) * | 2016-10-08 | 2017-03-08 | 江苏大学 | A kind of bismuth sulfide classifying nano flower electrode material for super capacitor and preparation method |
-
2017
- 2017-06-27 CN CN201710502025.5A patent/CN107308957B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105800687A (en) * | 2016-04-28 | 2016-07-27 | 江苏大学 | Method for preparing bismuth sulfide nanorod |
| CN106477629A (en) * | 2016-10-08 | 2017-03-08 | 江苏大学 | A kind of bismuth sulfide classifying nano flower electrode material for super capacitor and preparation method |
Non-Patent Citations (2)
| Title |
|---|
| QI ZHANG,ET.AL.: "In-situ room-temperature synthesis of amorphous/crystalline contact Bi2S3/Bi2WO6 heterostructures for improved photocatalytic ability", 《CERAMICS INTERNATIONAL》 * |
| 孙广: "纳米Bi2WO6空心球的制备及光学性能", 《河南科技大学学报：自然科学版》 * |
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| CN108355678A (en) * | 2018-03-09 | 2018-08-03 | 南昌航空大学 | A kind of compound micron bouquet of artificial gold-bismuth tungstate and its preparation method and application |
| CN108394956A (en) * | 2018-04-09 | 2018-08-14 | 沈阳化工大学 | A method of degradation antibiotic Ciprofloxacin Hydrochloride |
| CN108607498A (en) * | 2018-05-23 | 2018-10-02 | 四川理工学院 | A kind of preparation method and application of the enhanced bismuth tungstate of absorption property |
| CN108946863A (en) * | 2018-08-08 | 2018-12-07 | 辽宁大学 | A method of ultrasonotomography antibiotic waste water is catalyzed using copper tungstate |
| CN108946863B (en) * | 2018-08-08 | 2021-11-30 | 辽宁大学 | Method for degrading antibiotic wastewater by using copper tungstate to catalyze and ultrasonically |
| CN109046323A (en) * | 2018-10-18 | 2018-12-21 | 盐城工学院 | A kind of visible light catalyst CQDs/Bi2WO6And its preparation method and application |
| CN111167478A (en) * | 2020-01-08 | 2020-05-19 | 湖北大学 | CdS-Bi2WO6Application of semiconductor Z-type heterojunction in photocatalytic degradation of ethylene |
| CN111167478B (en) * | 2020-01-08 | 2022-08-30 | 湖北大学 | CdS-Bi 2 WO 6 Application of semiconductor Z-type heterojunction in photocatalytic degradation of ethylene |
| CN111203239A (en) * | 2020-02-27 | 2020-05-29 | 齐鲁工业大学 | Bismuth tungstate/bismuth sulfide/molybdenum disulfide heterojunction ternary composite material and preparation method and application thereof |
| CN111203239B (en) * | 2020-02-27 | 2021-05-28 | 齐鲁工业大学 | Bismuth tungstate/bismuth sulfide/molybdenum disulfide heterojunction ternary composite material and preparation method and application thereof |
| WO2021169196A1 (en) * | 2020-02-27 | 2021-09-02 | 齐鲁工业大学 | Bismuth tungstate/bismuth sulfide/molybdenum disulfide ternary heterojunction composite material, preparation method therefor, and application thereof |
| CN113235124A (en) * | 2021-05-18 | 2021-08-10 | 西北师范大学 | S-FeOOH/bismuth vanadate composite photo-anode and preparation method thereof |
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