CN108821339A - A kind of bismuthyl carbonate nanometer plate and preparation method thereof with photocatalysis performance - Google Patents
A kind of bismuthyl carbonate nanometer plate and preparation method thereof with photocatalysis performance Download PDFInfo
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- CN108821339A CN108821339A CN201810762292.0A CN201810762292A CN108821339A CN 108821339 A CN108821339 A CN 108821339A CN 201810762292 A CN201810762292 A CN 201810762292A CN 108821339 A CN108821339 A CN 108821339A
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- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 title claims abstract description 38
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 28
- 239000000725 suspension Substances 0.000 claims abstract description 24
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 18
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 16
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 16
- 239000001119 stannous chloride Substances 0.000 claims abstract description 16
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 14
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000004321 preservation Methods 0.000 claims abstract description 7
- 238000009826 distribution Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 231100001261 hazardous Toxicity 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 8
- 235000019441 ethanol Nutrition 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 7
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
- 238000002242 deionisation method Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
- C01G29/006—Compounds containing, besides bismuth, two or more other elements, with the exception of oxygen or hydrogen
-
- 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
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The bismuthyl carbonate nanometer plate and preparation method thereof with photocatalysis performance that the invention discloses a kind of adds stannous chloride and is combined, be nanometer disc-like particles, particle diameter distribution is in 5-25 nm using bismuth nitrate, sodium bicarbonate as primary raw material；Preparation method includes the following steps：（1）With the molar ratio of bismuth nitrate, sodium bicarbonate for 2：1 amount weighs raw material, is added to the water, and stirs evenly, then by bismuth nitrate and stannous chloride molar ratio 100：Stannous chloride is added in the ratio of 1-50, stirs evenly, obtains suspension；（2）The suspension is placed in reaction kettle, 100-200 DEG C of heat preservation 5-15 h is reacted；（3）After the reaction was completed, cooled to room temperature filters product, is centrifuged, washing, is dried at 40-80 DEG C to get bismuthyl carbonate nanometer plate is arrived.Nanometer plate bismuthyl carbonate of the invention does not add any organic solvent during the preparation process, non-hazardous to environment and human body；And process is simple, mild condition, production cost is low, it is easy to accomplish industrialization is suitable for promoting the use of.
Description
Technical field
The invention belongs to catalysis material technical fields, and in particular to a kind of bismuthyl carbonate nanometer with photocatalysis performance
Disk and preparation method thereof.
Background technique
Currently, the pollution of waste water from dyestuff is because it is big with discharge amount, coloration is high, complicated component, corruption in the pollution of industry
The feature that corrosion is strong, toxicity is big, the problem always being in waste water treatment.Not only the period is longer for traditional processing method, expense
Height, cost is big, and consumes a large amount of manpower and material resources, therefore is badly in need of seeking new administering method.
Since Fujishima in 1972 and Honda have found titanium dioxide under conditions of illumination（TiO2）It can be on particle
Since making water that redox reaction occur, the features such as Photocatalitic Technique of Semiconductor is without secondary pollution with Tai Yang Neng ﹑ with its Li, causes
The concern of global numerous scholars.Recently, it with the development and progress of photochemistry and technology, is eliminated in environment using photochemical catalyst
The research of various pollutants caused the extensive concern of people.Currently, conductor photocatalysis has been considered as eliminating environmental pollution
The most potential approach with value of object, moreover, having there is a large amount of photochemical catalyst to be developed.However, traditional photochemical catalyst,
Such as wherein most representational material TiO2Only to ultraviolet light photocatalytic activity with higher, urging under visible light
It is lower to change activity, therefore, there are great demands for new material of the people to exploitation visible light with highlight catalytic active.
The Chinese patent application of application number CN2013102257260 discloses a kind of high activity TiO2Nanometer plate photochemical catalyst
Synthetic method, water is mixed with glacial acetic acid, hydrofluoric acid first；Add mechanical stirring 10min after butyl titanate；It will be above-mentioned
Solution is put into 180 DEG C of hydro-thermals of reaction kettle for 24 hours；Then precipitation and separation, by precipitating with water centrifuge washing 3 times, 60 DEG C of dryings, 600 DEG C
Calcine 2h；Cooled to room temperature to get.TiO prepared by the present invention2Photocatalytic activity is relatively high, but only under ultraviolet light
There is higher photocatalytic activity, adaptation range is narrow.
The Chinese patent application of application number CN2014107535106 discloses a kind of composite photo-catalyst In2O3/ CNB and its
Preparation method weighs itrogenous organic substance and boron-containing compound respectively first, dissolves after mixing, then removes the solvent in mixture,
The solid calcining obtained after solvent will be removed, it is cooling, CNB is made；Weigh In respectively again2O3And CNB, crush, calcine after mixing,
It is cooling, obtain composite photo-catalyst.Calcine technology is used continuously in preparation process of the present invention, and calcine technology typical temperature is very
Height, reaction condition is more demanding and energy consumption is big, high production cost.
Summary of the invention
For the deficiency of existing issue, the bismuthyl carbonate nanometer with photocatalysis performance that the object of the present invention is to provide a kind of
Disk and preparation method thereof；The present invention can be realized the degradation to methylene blue under visible light, and degradation rate is up to 98%, and raw material valence
Lattice are cheap, reaction condition temperature, lower production costs.
The technical solution used to solve the technical problems of the present invention is that：
A kind of bismuthyl carbonate nanometer plate with photocatalysis performance adds protochloride using bismuth nitrate, sodium bicarbonate as primary raw material
Tin is combined, and is nanometer disc-like particles, and particle diameter distribution is mainly distributed on 7-13 nm in 5-25 nm.
A kind of preparation method of the bismuthyl carbonate nanometer plate with photocatalysis performance, includes the following steps：
（1）Molar ratio according to bismuth nitrate, sodium bicarbonate is 2：1 weighs raw material, is added to the water, and stirs evenly, then presses bismuth nitrate
With stannous chloride molar ratio 100：Stannous chloride is added in the ratio of 1-50, stirs evenly, obtains suspension；
（2）The suspension is placed in reaction kettle, 100-200 DEG C of heat preservation 5-15 h is reacted；
（3）After the reaction was completed, cooled to room temperature filters product, is centrifuged, washing, at 40-80 DEG C drying to get
To bismuthyl carbonate nanometer plate.
Step described in optimal technical scheme as the application（1）The quality of middle bismuth nitrate and water and volume ratio are 2：80-
100；Solvent is controlled in reasonable range, helps to improve reaction efficiency, while reducing the usage amount of solvent.
Preferably, the step（1）The compactedness of middle reaction kettle is 30-80%.
As the optimal technical scheme of the application, the step（2）It is middle that suspension is transferred in autoclave, 100-
200 DEG C of heat preservation 5-15 h are reacted.Under the reaction conditions, the bismuthyl carbonate nanometer plate tactical rule of preparation, uniform and shape
Looks controllability is strong.
As the optimal technical scheme of the application, the step（2）It is middle that suspension is transferred in autoclave, then move
Into thermostatic drying chamber, 100-200 DEG C of heat preservation 5-15 h is reacted；It is first transferred to autoclave, then moves to freeze-day with constant temperature
In case, better heat insulation effect can achieve.
As the optimal technical scheme of the application, the step（3）Deionized water is selected in middle washing, and ethyl alcohol respectively washs 3-5
It is secondary.
As the optimal technical scheme of the application, the step（3）Select centrifugal separator in 5000-10000 rpm, from
The heart time is 5-10 min.
Bismuthyl carbonate nanometer plate and preparation method thereof provided by the invention with photocatalysis performance, with prior art phase
Than having the advantages that：
（1）Reaction condition of the present invention is mild, lower to reaction condition requirement, and energy consumption is few, and production cost is low；
（2）The method provided by the invention for preparing bismuthyl carbonate nanometer plate is using bismuth nitrate, sodium bicarbonate as primary raw material, with water
It is raw materials used cheap for solvent, and do not add any organic solvent during the preparation process, it is non-hazardous to environment and human body；
（3）It is evenly distributed using bismuthyl carbonate nanometer panel surface prepared by the method for the present invention, form is good, gained bismuthyl carbonate material
Photocatalytic activity is more than 98% to material under visible light, than the photocatalytic activity of stannous chloride not being added to improve 39%.
Detailed description of the invention
Fig. 1 is the SEM figure of bismuthyl carbonate nanometer plate in embodiment 1.
Specific embodiment
The present invention is described in further details with reference to embodiments.Production is not specified in agents useful for same or instrument and equipment
Manufacturer, it is accordingly to be regarded as the conventional products that can be bought by market.
Embodiment 1
Five water bismuth nitrates, 0.73 g, 0.1 g of sodium bicarbonate are weighed, according to bismuth nitrate and stannous chloride molar ratio 100：1 weighs chlorine
Change stannous, is dissolved in 40 mL distilled water, stirs evenly, obtain suspension；Above-mentioned suspension is transferred to the height that volume is 100 mL
It presses in reaction kettle, which is placed in thermostatic drying chamber and keeps the temperature 10 h under the conditions of temperature is 140 DEG C, after the reaction was completed
By reaction kettle cooled to room temperature, product being filtered and is precipitated, 8000rpm is centrifuged 5min, after centrifugation twice, deionization
Water, 95% ethyl alcohol cross washing 3 times, are placed in 40-80 DEG C of drying, and it is 0.56g that gained bismuthyl carbonate quality is weighed after drying.
It accurately weighs 0.03 g tin dope bismuthyl carbonate, is added in the methylene blue that 30 mL concentration are 10 mg/L, can
Under light-exposed irradiation, 60 min, photocatalytic activity 98% are reacted.
Utilize Quanta200 type scanning electron microscope（FEI Co., Ltd）To prepare the pattern of bismuthyl carbonate material into
Row characterization, is shown in Fig. 1, it can be seen from the figure that its microscopic appearance is nanometer disc-like particles, particle diameter distribution is 5-25 nm, and surface
It is evenly distributed, form is good.
Embodiment 2
Five water bismuth nitrates, 0.73 g, 0.1 g of sodium bicarbonate are weighed, according to bismuth nitrate and stannous chloride molar ratio 100：10 weigh chlorine
Change stannous, is dissolved in 40 mL distilled water, stirs evenly, obtain suspension；Above-mentioned suspension is transferred to the height that volume is 100 mL
It presses in reaction kettle, which is placed in thermostatic drying chamber and keeps the temperature 10 h under the conditions of temperature is 120 DEG C, after the reaction was completed
By reaction kettle cooled to room temperature, product being filtered and is precipitated, 8000rpm is centrifuged 5min, after centrifugation twice, deionization
Water, 95% ethyl alcohol cross washing 3 times, are placed in 40-80 DEG C of drying, and it is 0.568 g that gained bismuthyl carbonate quality is weighed after drying.
It accurately weighs 0.03 g tin dope bismuthyl carbonate, is added in the methylene blue that 30 mL concentration are 10 mg/L, can
Under light-exposed irradiation, 60 min, photocatalytic activity 95% are reacted.
Embodiment 3
Five water bismuth nitrates, 0.73 g, 0.1 g of sodium bicarbonate are weighed, according to bismuth nitrate and stannous chloride molar ratio 100：20 weigh chlorine
Change stannous, is dissolved in 40 mL distilled water, stirs evenly, obtain suspension；Above-mentioned suspension is transferred to the height that volume is 100 mL
It presses in reaction kettle, which is placed in thermostatic drying chamber and keeps the temperature 5 h under the conditions of temperature is 140 DEG C, after the reaction was completed will
Reaction kettle cooled to room temperature, filters product and is precipitated, and 8000rpm is centrifuged 5min, after centrifugation twice, deionized water,
95% ethyl alcohol cross washing 3 times, is placed in 40-80 DEG C of drying, and it is 0.572 g that gained bismuthyl carbonate quality is weighed after drying.
It accurately weighs 0.03 g tin dope bismuthyl carbonate, is added in the methylene blue that 30 mL concentration are 10 mg/L, can
Under light-exposed irradiation, 60 min, photocatalytic activity 92% are reacted.
Embodiment 4
Five water bismuth nitrates, 0.73 g, 0.1 g of sodium bicarbonate are weighed, according to bismuth nitrate and stannous chloride molar ratio 100：30 weigh chlorine
Change stannous, is dissolved in 40 mL distilled water, stirs evenly, obtain suspension；Above-mentioned suspension is transferred to the height that volume is 100 mL
It presses in reaction kettle, which is placed in thermostatic drying chamber and keeps the temperature 8 h under the conditions of temperature is 100 DEG C, after the reaction was completed will
Reaction kettle cooled to room temperature, filters product and is precipitated, and 8000 rpm are centrifuged 7 min, after centrifugation twice, deionization
Water, 95% ethyl alcohol cross washing 3 times, are placed in 40-80 DEG C of drying, and it is 0.5652 g that gained bismuthyl carbonate quality is weighed after drying.
It accurately weighs 0.03 g tin dope bismuthyl carbonate, is added in the methylene blue that 30 mL concentration are 10 mg/L, can
Under light-exposed irradiation, 60 min, photocatalytic activity 90% are reacted.
Embodiment 5
Five water bismuth nitrates, 0.73 g, 0.1 g of sodium bicarbonate are weighed, according to bismuth nitrate and stannous chloride molar ratio 100：40 weigh chlorine
Change stannous, is dissolved in 40 mL distilled water, stirs evenly, obtain suspension；Above-mentioned suspension is transferred to the height that volume is 100 mL
It presses in reaction kettle, which is placed in thermostatic drying chamber and keeps the temperature 12 h under the conditions of temperature is 200 DEG C, after the reaction was completed
By reaction kettle cooled to room temperature, product being filtered and is precipitated, 10000rpm is centrifuged 5min, after being centrifuged 3 times, deionization
Water, 95% ethyl alcohol cross washing 3 times, are placed in 40-80 DEG C of drying, and it is 0.5683 g that gained bismuthyl carbonate quality is weighed after drying.
It accurately weighs 0.03 g tin dope bismuthyl carbonate, is added in the methylene blue that 30 mL concentration are 10 mg/L, can
Under light-exposed irradiation, 60 min, photocatalytic activity 95% are reacted.
Embodiment 6
Five water bismuth nitrates, 0.73 g, 0.1 g of sodium bicarbonate are weighed, according to bismuth nitrate and stannous chloride molar ratio 100：50 weigh chlorine
Change stannous, is dissolved in 40 mL distilled water, stirs evenly, obtain suspension；Above-mentioned suspension is transferred to the height that volume is 100 mL
It presses in reaction kettle, which is placed in thermostatic drying chamber and keeps the temperature 15 h under the conditions of temperature is 150 DEG C, after the reaction was completed
By reaction kettle cooled to room temperature, product being filtered and is precipitated, 5000rpm is centrifuged 10min, after centrifugation twice, deionization
Water, 95% ethyl alcohol cross washing 5 times, are placed in 40-80 DEG C of drying, and it is 0.569 g that gained bismuthyl carbonate quality is weighed after drying.
It accurately weighs 0.03 g tin dope bismuthyl carbonate, is added in the methylene blue that 30 mL concentration are 10 mg/L, can
Under light-exposed, 60 min, photocatalytic activity 96% are reacted.
Control group：
Five water bismuth nitrates, 0.73 g, 0.1 g of sodium bicarbonate are weighed, is dissolved in 40 mL distilled water, is stirred evenly, obtain suspension；It will
Above-mentioned suspension is transferred to volume as in the autoclave of 100 mL, which is placed in thermostatic drying chamber
10 h are kept the temperature under the conditions of 140 DEG C, after the reaction was completed by reaction kettle cooled to room temperature, product are filtered and is precipitated,
8000rpm is centrifuged 5min, and after centrifugation twice, deionized water, 95% ethyl alcohol cross washing 3 times are placed in 40-80 DEG C of drying, drying
Weighing gained bismuthyl carbonate quality afterwards is 0.56 g.
It accurately weighs 0.03 g control group bismuthyl carbonate, is added in the methylene blue that 30 mL concentration are 10 mg/L, can
Under light-exposed irradiation, 60 min are reacted, photocatalytic activity 59%, compared with the control group, the photocatalysis of bismuthyl carbonate of the present invention drop
Solution rate is up to 98% than the photocatalytic activity of stannous chloride not being added to improve 39 percentage points.
Protection content of the invention is not limited to above embodiments.Without departing from the spirit and scope of the invention, originally
Field technical staff it is conceivable that variation and advantage be all included in the present invention, and with the attached claims be protection
Range.
Claims (5)
1. a kind of bismuthyl carbonate nanometer plate with photocatalysis performance, which is characterized in that with bismuth nitrate, sodium bicarbonate be main former
Material adds stannous chloride and is combined, is nanometer disc-like particles, particle diameter distribution is in 5-25 nm.
2. the preparation method of the bismuthyl carbonate nanometer plate described in claim 1 with photocatalysis performance, which is characterized in that including
Following steps：
（1）Molar ratio according to bismuth nitrate, sodium bicarbonate is 2：1 weighs raw material, is added to the water, and stirs evenly, then presses bismuth nitrate
With stannous chloride molar ratio 100：Stannous chloride is added in the ratio of 1-50, stirs evenly, obtains suspension；
（2）The suspension is placed in reaction kettle, 100-200 DEG C of heat preservation 5-15 h is reacted；
（3）After the reaction was completed, cooled to room temperature filters product, is centrifuged, washing, at 40-80 DEG C drying to get
To bismuthyl carbonate nanometer plate.
3. the preparation method of the bismuthyl carbonate nanometer plate according to claim 2 with photocatalysis performance, which is characterized in that
The step（1）The quality of bismuth nitrate and water and volume ratio are 2：80-100.
4. the preparation method of the bismuthyl carbonate nanometer plate according to claim 2 with photocatalysis performance, which is characterized in that
The step（2）Middle that suspension is transferred in autoclave, 100-200 DEG C of heat preservation 5-15 h is reacted.
5. the preparation method of the bismuthyl carbonate nanometer plate according to claim 4 with photocatalysis performance, which is characterized in that
The step（2）It is middle that suspension is transferred in autoclave, it then moves in thermostatic drying chamber, 100-200 DEG C of heat preservation 5-15
H is reacted.
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| CN110813342A (en) * | 2019-11-26 | 2020-02-21 | 大连工业大学 | Preparation method of cobaltosic oxide-doped bismuthyl carbonate catalyst |
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