CN108479815B - A kind of BiOCl photochemical catalyst octahedronlike and the preparation method and application thereof - Google Patents
A kind of BiOCl photochemical catalyst octahedronlike and the preparation method and application thereof Download PDFInfo
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000003054 catalyst Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000015556 catabolic process Effects 0.000 claims abstract description 21
- 238000006731 degradation reaction Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 15
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 claims abstract description 13
- 239000002608 ionic liquid Substances 0.000 claims abstract description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- 238000002525 ultrasonication Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 12
- 229940012189 methyl orange Drugs 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 239000000985 reactive dye Substances 0.000 claims description 9
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 7
- 229940043267 rhodamine b Drugs 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000001154 acute effect Effects 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 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 abstract description 4
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 description 18
- 239000000975 dye Substances 0.000 description 13
- 238000007146 photocatalysis Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000003344 environmental pollutant Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 231100000719 pollutant Toxicity 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000013210 evaluation model Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
-
- 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
- B01J27/06—Halogens; Compounds thereof
-
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/41—Particle morphology extending in three dimensions octahedron-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of BiOCl photochemical catalysts octahedronlike and the preparation method and application thereof, belong to the preparation technical field of catalysis material, which is characterized in that weigh five nitric hydrate bismuths and are dispersed in ethylene glycol, obtain clear solution under ultrasonication.It is slowly added dropwise ionic liquid [BMIM] Cl, it is vigorously stirred 24 h, solution is fully transferred in the stainless steel autoclave that liner is polytetrafluoroethylene (PTFE), autoclave is placed in 160 DEG C of -180 DEG C of 4 h-12h of reaction in baking oven, after cooled to room temperature, product is centrifugated, then is cleaned respectively with dehydrated alcohol and secondary water, the solid being collected into is placed in 80 DEG C of dry 8h in baking oven, BiOCl octahedronlike can be obtained.The synthetic method is easy to operate, at low cost, and products therefrom has single-phase simple tetragonal crystalline structure, has remarkable result to the degradation of industrial dye.
Description
Technical field:
The invention belongs to the preparation technical fields of catalysis material, are provided in particular in a kind of BiOCl photocatalysis octahedronlike
Agent and the preparation method and application thereof.
Background technique:
With the fast development of human society, energy shortage and problem of environmental pollution more and more influence and threaten people
The survival and development of class.Wherein dye wastewater has the characteristics that color depth, complicated component, COD value are high and difficult to degrade, to ecology
Environment and human health life bring serious harm, and therefore, efficiently removing dye wastewater has important research meaning.Currently, place
There are many method for managing dye wastewater, such as membrane separation process, absorption method, electrochemical oxidation process, photocatalytic oxidation, ultrasonic degradation
Deng.Wherein, photocatalytic degradation method utilizes clean reproducible energy solar energy, the thorough degradation of dyestuff contaminant is realized, due to it
It is widely used in environmental pollution with advantages such as efficient dyestuff contaminant degradation property, environmentally protective, economically feasibles and controls
Reason.The key of photocatalysis technology is the preparation of photochemical catalyst, thus improves photocatalysis utilization efficiency and develop the light of efficient stable
Catalysis material becomes the research hotspot of photocatalysis field.
Bismuthyl chloride (BiOCl) belongs to a kind of multicomponent semiconductor of V-VI-VII main group, due to special layer structure
With appropriately sized forbidden bandwidth, excellent optics, electricity, magnetics, fluorescence and catalytic performance with unique.Bi in BiOCl
The 6s of atom and the 2p track bonding of O atom, affect the valence band of semiconductor and the composition of conduction band, make its light abstraction width to can
Light-exposed area's extension, while there is good photocatalysis stability, therefore BiOCl photochemical catalyst has obtained the concern of researcher.Such as
Liu et al. is chlorine source and template direction agent using hexadecyltrimethylammonium chloride, is prepared for two-dimentional plate-like using microwave-hydro-thermal method
BiOCl nanometer sheet and three-dimensional porous flower ball-shaped BiOCl aggregation, in visible light photocatalytic degradation rhodamine B and mixed dye (Luo Dan
Bright B and methyl orange) show high photocatalytic activity, and the photocatalysis performance of three-dimensional porous flower ball-shaped BiOCl it is more preferable (R.Liu,
et al.,New J.Chem.,2018,42,137-149.).Such as Zheng is prepared in SBA-16 caged hole using the precipitation method
Quantum size BiOCl, the average diameter of BiOCl particle are decreased to 6.1nm, to the light of methyl orange under simulated solar irradiation irradiation
Catalytic degradation has high activity (Y.Zheng, et al., Mater.Lett., 2017,205,236-239.).Such as Tian is used
Solvent-thermal method is prepared for the BiOCl tiny balloon constructed by the thin BiOCl nanometer sheet with (001) crystal face, in surfactant
Under the regulation of polyvinylpyrrolidone, the pattern of product is changed from solid microsphere to tiny balloon, in visible light photocatalytic degradation sieve
In red bright B experiment, show high photocatalytic activity and stability (Y.Tian, et al.J.Nanosci.Nanotechnol.,
2017,17(9),6328-6336.)。
It is well known that closely related, the BiOCl photocatalysis such as the physics of material, chemical property and its pattern, size and structure
The appearance structure of agent has a major impact its photocatalysis performance.The present invention is using five nitric hydrate bismuths as bismuth source, ionic liquid
[BMIM] Cl is chlorine source, and ethylene glycol is solvent, it is not necessary that any other additive is added, is prepared for using solvent-thermal method octahedronlike
BiOCl.Product morphology is uniform, good dispersion, does not occur agglomeration, special crystal structure, makes BiOCl photochemical catalyst can
Light-exposed catalytic field shows excellent application potential.
Summary of the invention:
The first aspect of the present invention has been designed to provide a kind of BiOCl photochemical catalyst octahedronlike, with uniform
Pattern, good dispersibility, special crystal structure, make it have good visible light catalytic performance.
The technical solution that the present invention takes to achieve the above object is as follows:
A kind of BiOCl photochemical catalyst octahedronlike, which is characterized in that photochemical catalyst BiOCl is powder, and crystal phase is simple
Tetragonal, pattern are octahedral structure, about 1 μm -5 μm of particle size.
The second aspect of the present invention purpose is to provide the preparation method of BiOCl octahedronlike a kind of, has simple process, easily
Operation, it is low in cost, it is high-efficient, activity it is good the advantages that.
The technical solution that the present invention takes to achieve the above object is as follows:
A kind of preparation method of BiOCl photochemical catalyst octahedronlike, which is characterized in that include the following steps:
(1) five nitric hydrate bismuth of precise 0.3mmol is dispersed in 20mL ethylene glycol, obtains clarifying under ultrasonication molten
Liquid.
(2) 0.1mmol-0.4mmol ionic liquid [BMIM] Cl is slowly added dropwise into the clear solution of step (1),
It is vigorously stirred for 24 hours.
(3) solution in step (2) is fully transferred to liner as (volume is filled out in the stainless steel autoclave of polytetrafluoroethylene (PTFE)
Filling rate is 80%), autoclave to be placed in 160 DEG C of -180 DEG C of reaction 4h-12h in baking oven.
(4) to after reaction, autoclave cooled to room temperature, then 5 are respectively cleaned with dehydrated alcohol and secondary water respectively
More than secondary, the solid being collected into is placed in 80 DEG C of dry 8h in baking oven, BiOCl octahedronlike can be obtained.
Preferably:
Ionic liquid [BMIM] Cl additional amount is 0.3mmol, and step (3) reaction temperature is 170 DEG C, reaction time 8h.
The third aspect of the present invention purpose is to provide a kind of BiOCl octahedronlike in degradation of dye pollutant, especially first
Application in base orange, rhodamine B, reactive dye etc..
Beneficial effects of the present invention are as follows:
(1) any other additive is not used in reaction process of the invention, reduces the production cost of material.
(2) synthetic method is simple to operation, reproducible, and raw material is cheap and easy to get.
(3) photochemical catalyst prepared by has micron-scale, is easy to be separated by solid-liquid separation in photocatalysis experiment, facilitates light and urge
The recycling and reusing of agent.
(4) compared with existing commercially available BiOCl, BiOCl octahedronlike of the invention, to industrial dye methyl orange,
The degradation efficiency of rhodamine B and various reactive dye increases substantially.
Detailed description of the invention:
Fig. 1 is scanning electron microscope (SEM) photo of product in embodiment 1；
Fig. 2 is scanning electron microscope (SEM) photo of product in embodiment 1；
Fig. 3 is the X-ray diffractogram (XRD) of product in embodiment 1；
Under visible light illumination for the BiOCl octahedronlike and BiOCl of purchase, the concentration of methyl orange solution is at any time by Fig. 4
Change curve；
Under visible light illumination for the BiOCl octahedronlike and BiOCl of purchase, the concentration of rhodamine B solution is at any time by Fig. 5
Change curve；
Fig. 6 is BiOCl octahedronlike and the BiOCl of purchase is through radiation of visible light 90min, and the degradation of various reactive dye is imitated
Fruit.
Specific embodiment:
Embodiment 1:
Five nitric hydrate bismuth of precise 0.3mmol is dispersed in 20mL ethylene glycol, obtains clear solution under ultrasonication.
It is slowly added dropwise 0.3mmol ionic liquid [BMIM] Cl, is vigorously stirred for 24 hours, it is polytetrafluoro that solution, which is fully transferred to liner,
In the stainless steel autoclave of ethylene (volumetric filling ratio 80%).Autoclave is placed in 170 DEG C of reaction 8h in baking oven, wait react knot
Shu Hou, autoclave cooled to room temperature, then respectively cleaned 5 times or more with dehydrated alcohol and secondary water respectively, consolidate what is be collected into
Body is placed in 80 DEG C of dry 8h in baking oven, can obtain BiOCl octahedronlike.
The examination and test of products:
The pattern that SEM result (Fig. 1 and Fig. 2) intuitively presents product is octahedral structure, and product morphology is uniform, disperses
Property is good, and size reaches micron order, and about 3 μm.XRD result (Fig. 3) and simple tetragonal structure BiOCl standard card (JCPDS
No.82-0485 it) coincide, shows that the crystal phase of product is simple tetragonal structure BiOCl.
Application Example:
Test object: BiOCl octahedronlike prepared by the embodiment of the present invention 1 and the BiOCl of commercially available purchase (are purchased from Zhengzhou
Rich hundred million Chemical Co., Ltd.s).
In order to study the photocatalytic activity of prepared product, with methyl orange aqueous solution of degrading, rhodamine B aqueous solution and various
Aqueous solution of reactive dye is evaluation model, as active yellow R-4RFN, active red R-2BF, Reactive dye red M-3BE, active golden yellow RHB and
Reactive blue RHB (the above dyestuff is bought from Zhejiang Province Runtu intercalated Co., Ltd).In order to compare, by etc. quality it is octahedronlike
The BiOCl and BiOCl 20mg directly bought, is added to 50mL 20mgL-1In dye solution, ultrasonic disperse obtains suspension, will
It is placed in dark place stirring 60min, to reach adsorption/desorption balance.Using 250W xenon lamp as light source, prolonged exposure, and when one section
Between sample, after centrifuge separation to clear solution with ultraviolet-visible spectrophotometer (UV-vis, UV-2550, Japanese Shimadzu) survey
Examination, the concentration for observing dyestuff change, and the concentration curve of methyl orange solution and rhodamine B solution is respectively such as Fig. 4 and Fig. 5 institute
Show.
Compare curve in figure it is found that BiOCl illumination 70min octahedronlike just makes various dyes under identical experiment condition
The degradation rate of material reaches 90%, and the BiOCl bought is only reached or close to 30%, and the degradation rate of BiOCl octahedronlike
Than the BiOCl of purchase.Under the action of catalyst, various reactive dye are after radiation of visible light 90min, various reactive dye
Degradation effect as shown in fig. 6, BiOCl octahedronlike to the degradation rate of various reactive dye more than 95%, and buy BiOCl
There are no more than 35%.Photocatalysis experimental data compares it is found that BiOCl octahedronlike is high to dyestuff degrading activity, speed is fast, table
Reveal superior visible light catalysis activity.
Alternative embodiment 2-26:
Dosage and other experiment items according to preparation method described in embodiment 1, using table 1 intermediate ion liquid [BMIM] Cl
BiOCl photochemical catalyst octahedronlike is prepared in part.And the BiOCl photochemical catalyst octahedronlike for preparing embodiment 2-26, point
It Ying Yongyu be catalyzed methyl orange solution, and it is as shown in table 1 to count its catalytic effect.
Table 1, the dosage of embodiment 2-26 intermediate ion liquid [BMIM] Cl and other experiment conditions and catalytic performance effect pair
According to
Analysis:
As shown above, under different technology conditions, the BiOCl photochemical catalyst octahedronlike of preparation, in photocatalytic activity
Aspect is variant.In general, in the identical situation of other conditions, with the increase of ionic liquid [BMIM] Cl additional amount,
The variation tendency gradually increased is presented to the degradation rate of pollutant methyl orange in product, when [BMIM] Cl additional amount is more than 0.3mmol
When, degradation rate increase is unobvious, shows the photocatalytic activity of methyl orange solution with the increase of ionic liquid [BMIM] Cl dosage
And increases and gradually tend towards stability.
In the identical situation of other conditions, with the raising of reaction temperature, degradation rate of the product to pollutant methyl orange
Presentation first increases the variation tendency reduced again.When reaction temperature is lower, product is to the degradation rate of pollutant methyl orange with reaction
The raising of temperature and increase, when reaction temperature is 170 DEG C, the degradation rate of methyl orange reaches maximum.Continue to increase reaction temperature,
Product reduces the degradation rate of methyl orange instead, this may be since reaction temperature is too high, the shape of octahedron homogeneity of product,
Surface texture, dispersibility etc. are deteriorated, and photocatalytic activity is caused slightly to reduce.
In the identical situation of other conditions, with the extension of reaction time, degradation rate of the product to pollutant methyl orange
Presentation first quicklys increase the variation tendency gradually to tend towards stability again.This may be due to the extension of reaction time, product
The homogeneity and dispersibility of shape of octahedron structure gradually increase and reach best, thus product to the degradation rate of methyl orange gradually
It increases, photocatalytic activity gradually increases, and finally tends towards stability.
Through counting, best synthetic technological condition are as follows: ionic liquid [BMIM] Cl additional amount is 0.3mmol, and reaction temperature is
170 DEG C, reaction time 8h, prepared properties of catalyst is best.
Claims (5)
1. a kind of BiOCl photochemical catalyst octahedronlike, which is characterized in that photochemical catalyst BiOCl is powder, and crystal phase is simple four
Square structure BiOCl standard card JCPDS No. 82-0485, pattern are octahedral structure, about 1 μm -5 μm of particle size.
2. a kind of preparation method of BiOCl photochemical catalyst octahedronlike described in claim 1, which is characterized in that including following step
It is rapid:
(1) it weighs 0.3 mmol, five nitric hydrate bismuth to be dispersed in 20 mL ethylene glycol, obtains clear solution under ultrasonication；
(2) mmol of 0.1 mmol~0.4 ionic liquid [BMIM] Cl is slowly added dropwise into the clear solution of step (1), it is acute
24 h of strong stirring；
(3) solution in step (2) is fully transferred in the stainless steel autoclave that liner is polytetrafluoroethylene (PTFE), autoclave is set
160 DEG C~180 DEG C reaction 4 h~12 h in baking oven；
(4) to after reaction, autoclave cooled to room temperature, then cleaned respectively with dehydrated alcohol and water, by what is be collected into
Solid is placed in 80 DEG C of 8 h of drying in baking oven, can obtain BiOCl octahedronlike.
3. a kind of preparation method of BiOCl photochemical catalyst octahedronlike according to claim 2, it is characterised in that: step
(1) in, disperse 0.3 mmol, five nitric hydrate bismuth using the method for ultrasound.
4. a kind of preparation method of BiOCl photochemical catalyst octahedronlike according to claim 2, it is characterised in that: ion
Liquid [BMIM] Cl additional amount is 0.3 mmol, and step (3) reaction temperature is 170 DEG C, and the reaction time is 8 h.
5. BiOCl photochemical catalyst octahedronlike described in a kind of claim 1 is in degradation methyl orange, rhodamine B and reactive dye
Using.
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| CN101186336A (en) * | 2007-12-05 | 2008-05-28 | 北京航空航天大学 | Method for preparing layer thickness homogenized bismuth oxyhalide |
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| CN105214694A (en) * | 2015-09-30 | 2016-01-06 | 南京大学 | A kind of soft template method prepares the method for BiOCl hollow shell |
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