CN107115857A - A kind of CQDs/ β Bi2O3Composite visible light catalyst and preparation method thereof - Google Patents
A kind of CQDs/ β Bi2O3Composite visible light catalyst and preparation method thereof Download PDFInfo
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- CN107115857A CN107115857A CN201710251115.1A CN201710251115A CN107115857A CN 107115857 A CN107115857 A CN 107115857A CN 201710251115 A CN201710251115 A CN 201710251115A CN 107115857 A CN107115857 A CN 107115857A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002131 composite material Substances 0.000 claims abstract description 30
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 117
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 72
- 229910001868 water Inorganic materials 0.000 claims description 38
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 32
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- -1 polytetrafluoroethylene Polymers 0.000 claims description 17
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000002604 ultrasonography Methods 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229960005070 ascorbic acid Drugs 0.000 claims description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims description 8
- 239000011668 ascorbic acid Substances 0.000 claims description 8
- 238000005352 clarification Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 230000003068 static effect Effects 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 239000010431 corundum Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 230000001788 irregular Effects 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 3
- 239000011941 photocatalyst Substances 0.000 abstract description 3
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 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 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- B01J35/39—
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B01J35/30—
-
- 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
- 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
Abstract
The invention discloses a kind of CQDs/ β Bi2O3Composite visible light catalyst and preparation method thereof, the composite visible light catalyst includes carbon quantum dot and Bi2O3Nanometer sheet.By the present invention in that with hydro-thermal method and polishing, that is, utilizing Bi2O2CO3It is used as Bi2O3Predecessor, Bi is prepared by high-temperature calcination2O3Nanometer sheet, is mixed by it with the carbon quantum dot prepared, grinds to prepare CQDs/ β Bi2O3Composite visible light catalyst.This composite photo-catalyst can strengthen upper converting photoluminescent behavior, so as to effectively improve the utilization rate of sunshine.It is an advantage of the invention that：Technique is simple, and controllability is good, and harmony is high.
Description
Technical field
The present invention relates to heterojunction photocatalyst and preparation method thereof, more particularly to a kind of CQDs/ β-Bi2O3It is compound visible
Photochemical catalyst and preparation method.
Background technology
With increasingly serious water pollution problems, semi-conducting material widely is used for studying in photocatalytic degradation water
Pollutant.And in recent decades, bismuthino nano material is more and more paid close attention to by researcher, because of its conduction band and valence band
All it is made up of s and p tracks, and special layer structure, light induced electron can be promoted to be migrated from valence band to conduction band, so as to reach
The purpose of photocatalytic pollutant degradation.But, after being excited due to material light, the recombination rate in electronics and hole is higher, therefore pole
The earth limits its application.In order to improve the photocatalysis efficiency of material, researcher is by the way that two kinds of bandgap structures are matched
Material is configured to composite, is effectively improved electronics and the separation rate in hole.
In 2004, since researcher obtains carbon quantum dot when preparing single-walled carbon nanotube by electrophoresis, because its is low
The advantages of cost, simple preparation and fluorescent both, carbon quantum dot widely is used for being combined with catalysis material, Ke Yiti
The separation rate of high photo-generated carrier, so as to reach the purpose of enhancing photocatalytic pollutant degradation.
The content of the invention
It is an object of the invention to provide one kind by carbon quantum dot and semiconductor Bi2O3Nanometer sheet be combined into CQDs/ β-
Bi2O3Composite visible light catalyst and preparation method thereof.
To reach above-mentioned purpose, CQDs/ β-Bi of the invention2O3Composite visible light catalyst, by carbon quantum of uniform size
Point is attached to Bi in irregular shape2O3Constituted in nanometer sheet.
The preparation method of the present invention is as follows：
1)Bi2O2CO3Preparation
By 1~3mmol Bi (NO3)3·5H2O ultrasounds, which are dissolved in 5~20mL dilute nitric acid solution, is sufficiently stirred for obtaining solution
A；
By 1~2mmol C6H8O7·H2O, which is added in solution A, is sufficiently stirred for obtaining settled solution B；
Be added dropwise with microsyringe into the solution B of clarification 2mol/L NaOH solution to the pH value of solution B for 4.0~
4.5；
Above-mentioned solution B is transferred in polytetrafluoroethylene (PTFE) water heating kettle, 24h is kept at 180 DEG C, with super after band reactor cooling
Pure water and absolute ethyl alcohol are respectively washed, and white product C i.e. Bi is obtained in drying at 80 DEG C2O2CO3；
2)β-Bi2O3Preparation
Take 1.0g products C to be uniformly layered in Noah's ark type corundum crucible, and be positioned over Muffle furnace, with 5 DEG C of heatings per minute
Speed is heated to 300~500 DEG C from room temperature, and keeps 2h, and it is β-Bi that product D is obtained after cooling2O3；
3) CQDs preparation
In the aqueous solution that 0.5~2.0g ascorbic acid is added to 10~30ml ethanol, it must clarify molten after ultrasound
Liquid E, solution E is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, 4h, Temperature fall is incubated at 160 DEG C
Afterwards brown solution F, with dichloromethane in separatory funnel to solution F extract and it is static after, collect upper solution bag filter
Brown viscous shape CQDs solution is obtained after dialysis；
4)CQDs/β-Bi2O3Preparation
Product D is transferred to after the CQDs solution stirring that 0.5ml, 1ml, 2ml, 3ml or 4ml are added in crucible, grinding, used
Water and washes of absolute alcohol, CQDs/ β-Bi are obtained in freeze-day with constant temperature at 60 DEG C2O3Composite visible light catalyst.
The aqueous solution of described ethanol is that ethanol presses 1 with water:The mixed solution of 1 volume ratio.
CQDs/ β-the Bi of the present invention2O3Photochemical catalyst is by carbon quantum dot and Bi2O3Nanometer sheet is stirred in aqueous
Grinding is mixed, is then dried, causes carbon quantum dot to be uniformly attached to Bi by annealing2O3On nanometer sheet surface, so as to form composite wood
Material, realizes efficiently separating for electron-hole when finally carrying out light-catalyzed reaction.
In light-catalyzed reaction, two kinds of materials are combined composition composite, are to reduce the compound one kind of photo-generated carrier
Effective ways.Bi2O3Although nanometer sheet can absorb visible ray, light excites the recombination rate in formed electronics and hole pair
It is higher, therefore to improve the efficiency of photocatalytic degradation, the present invention is by by carbon quantum dot and Bi2O3Nanometer sheet is combined, i.e., sharp
Carbon quantum dot is set to be attached to Bi with polishing2O3CQDs/ β-Bi are prepared in nanometer sheet2O3Composite visible light catalyst.It is described multiple
Condensation material refers to Bi2O3Light excite after, the carrier of formation can be transferred in carbon quantum dot, in Bi2O3Nanometer sheet and carbon
The interface of quantum dot can form activated centre, wherein the pollutant that the active material generated can be effectively in degradation water, realize β-
Bi2O3Interior electronics and hole are efficiently separated, so as to improve the photocatalysis efficiency of material.Ensureing Bi2O3Still there is suction to visible ray
In the case of receipts, additionally it is possible to enable the composite catalyst that visible absorption scope is broadened and electronics and hole are efficiently separated.
The present invention prepares CQDs/ β-Bi using wet chemical method2O3Composite visible light catalyst, technique is simple, controllability
Good, harmony is high.
Brief description of the drawings
Fig. 1 is CQDs/ β-Bi prepared by the present invention2O3The scanned picture of composite visible light catalyst and the distribution of Elements C
Figure, wherein a CQDs/ β-Bi2O3The projection electron microscope of composite visible light catalyst, (stain is CQD, and sheet is β-Bi2O3)、b
For CQDs/ β-Bi2O3The Elemental redistribution total figure of composite visible light catalyst, c are that C element distribution map, d are Bi distribution diagram of element, e
For O distribution diagram of element.
Fig. 2 is the CQDs/ β-Bi under visible ray photograph2O3Composite visible light catalyst, β-Bi2O3With β-Bi2O3- CQDs is (right
Ratio) to the degradation curve of rhodamine B, wherein abscissa is the time, when ordinate is certain moment t, the degraded concentration C of rhodamine
With initial concentration C0Ratio.
Embodiment
Embodiment 1：
1)Bi2O2CO3Preparation
By 1.5mmol Bi (NO3)3·5H2O ultrasounds, which are dissolved in 10mL dilute nitric acid solution, is sufficiently stirred for obtaining solution A；
By 1.5mmol C6H8O7·H2O, which is added in solution A, is sufficiently stirred for obtaining settled solution B；
The pH value that 2mol/L NaOH solution to solution B is added dropwise into the solution B of clarification with microsyringe is 4.12；
Above-mentioned solution B is transferred in polytetrafluoroethylene (PTFE) water heating kettle, 24h is kept at 180 DEG C, with super after band reactor cooling
Pure water and absolute ethyl alcohol are respectively washed 3 times, and white product C i.e. Bi is obtained in drying at 80 DEG C2O2CO3；
2)β-Bi2O3Preparation
Take 1.0g products C to be uniformly layered in Noah's ark type corundum crucible, and be positioned over Muffle furnace, with 5 DEG C of heatings per minute
Speed is heated to 350 DEG C from room temperature, and keeps 2h, and it is β-Bi that product D is obtained after cooling2O3；
3) CQDs preparation
1g ascorbic acid is added to 25ml ethanol and water by 1:In the aqueous solution of the ethanol of 1 volume ratio mixing,
Settled solution E is obtained after ultrasound, solution E is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, at 160 DEG C
Be incubated 4h, after Temperature fall brown solution F, in separatory funnel solution F is extracted with dichloromethane and it is static after, in collection
Layer solution obtains brown viscous shape CQDs solution after being dialysed with bag filter；
4)CQDs/β-Bi2O3Preparation
Product D is transferred to after the CQDs solution stirring that 2ml is added in crucible, grinding, with water and washes of absolute alcohol, in
Freeze-day with constant temperature obtains CQDs/ β-Bi at 60 DEG C2O3- 2 composite visible light catalysts.
Prepared CQDs/ β-Bi as seen from Figure 12O3In composite visible light catalyst, carbon quantum dot is uniformly adhered to
Bi2O3In nanometer sheet, and the distribution map of Elements C demonstrates the well-proportioned distribution of carbon quantum dot in the composite.
Comparative example
1)Bi2O2CO3Preparation
By 1.5mmol Bi (NO3)3·5H2O ultrasounds are dissolved in 10mL dilute nitric acid solution, and 1.5h is stirred at room temperature, and obtain molten
Liquid A；1.5mmol C will be added6H8O7·H2O is added in solution A, is stirred 0.5h, is obtained settled solution B；Use microsyringe
2M NaOH are added dropwise into the solution B of clarification, the pH to solution is 4.12.Above-mentioned solution B is transferred to polytetrafluoroethylene (PTFE) water heating kettle
In, 24h is kept at 180 DEG C, is respectively washed after band reactor cooling with ultra-pure water and absolute ethyl alcohol at 3 times, 80 DEG C and dries 3h, obtained
To white product C；
2) CQDs preparation
1.0g ascorbic acid is added in 25ml ethanol-water solution (v:V=1:1).Obtain clear after ultrasound through 2h
Clear solution E, solution is transferred in the stainless steel autoclave that 50ml polytetrafluoroethylene (PTFE) is liner, 4h is incubated at 160 DEG C,
Brown solution E is obtained after Temperature fall.With dichloromethane in separatory funnel to solution E extracted several times, after static 24 hours, collect
After upper solution is dialysed 24 hours with bag filter, brown viscous shape product F is obtained.
3)β-Bi2O3- CQDs preparation
1.0g product C is transferred in crucible, 2ml CQDs solution is added, labeled as β-Bi2O3-CQDs.By sample
It is stirred and grinds after 1h, freeze-day with constant temperature 6 hours, is finally positioned over Muffle at 60 DEG C with water and washes of absolute alcohol for several times
In stove, 350 DEG C are heated to 5 DEG C of heating rates per minute, and keeps 2h, product β-Bi are obtained after cooling2O3-CQDs。
Embodiment 1 and comparative example are subjected to photocatalysis performance test, contrast as seen from Figure 2 is prepared by high-temperature calcination
β-Bi2O3- CQDs composite photo-catalysts, β-Bi2O3- CQDs materials, CQDs/ β-Bi2O3Composite visible light catalyst is shown
Best photocatalysis performance.
Embodiment 2：
1)Bi2O2CO3Preparation
By 1mmol Bi (NO3)3·5H2O ultrasounds, which are dissolved in 10mL dilute nitric acid solution, is sufficiently stirred for obtaining solution A；
By 1.3mmol C6H8O7·H2O, which is added in solution A, is sufficiently stirred for obtaining settled solution B；
The pH value that 2mol/L NaOH solution to solution B is added dropwise into the solution B of clarification with microsyringe is 4.12；
Above-mentioned solution B is transferred in polytetrafluoroethylene (PTFE) water heating kettle, 24h is kept at 180 DEG C, with super after band reactor cooling
Pure water and absolute ethyl alcohol are respectively washed 3 times, and white product C i.e. Bi is obtained in drying at 80 DEG C2O2CO3；
2)β-Bi2O3Preparation
Take 1.0g products C to be uniformly layered in Noah's ark type corundum crucible, and be positioned over Muffle furnace, with 5 DEG C of heatings per minute
Speed is heated to 430 DEG C from room temperature, and keeps 2h, and it is β-Bi that product D is obtained after cooling2O3；
3) CQDs preparation
1.5g ascorbic acid is added to 20ml ethanol and water by 1:The aqueous solution of the ethanol of 1 volume ratio mixing
In, settled solution E is obtained after ultrasound, solution E is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, 160
Brown solution F is incubated after 4h, Temperature fall to obtain at DEG C, in separatory funnel solution F is extracted with dichloromethane and it is static after, receive
Collection upper solution obtains brown viscous shape CQDs solution after being dialysed with bag filter；
4)CQDs/β-Bi2O3Preparation
Product D is transferred to after the CQDs solution stirring that 0.5ml is added in crucible, grinding, with water and washes of absolute alcohol,
CQDs/ β-Bi are obtained in freeze-day with constant temperature at 60 DEG C2O3- 0.5 composite visible light catalyst.
Embodiment 3：
1)Bi2O2CO3Preparation
By 2mmol Bi (NO3)3·5H2O ultrasounds, which are dissolved in 5mL dilute nitric acid solution, is sufficiently stirred for obtaining solution A；
By 2mmol C6H8O7·H2O, which is added in solution A, is sufficiently stirred for obtaining settled solution B；
The pH value that 2mol/L NaOH solution to solution B is added dropwise into the solution B of clarification with microsyringe is 4.0；
Above-mentioned solution B is transferred in polytetrafluoroethylene (PTFE) water heating kettle, 24h is kept at 180 DEG C, with super after band reactor cooling
Pure water and absolute ethyl alcohol are respectively washed 3 times, and white product C i.e. Bi is obtained in drying at 80 DEG C2O2CO3；
2)β-Bi2O3Preparation
Take 1.0g products C to be uniformly layered in Noah's ark type corundum crucible, and be positioned over Muffle furnace, with 5 DEG C of heatings per minute
Speed is heated to 300 DEG C from room temperature, and keeps 2h, and it is β-Bi that product D is obtained after cooling2O3；
3) CQDs preparation
0.5g ascorbic acid is added to 10ml ethanol and water by 1:The aqueous solution of the ethanol of 1 volume ratio mixing
In, settled solution E is obtained after ultrasound, solution E is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, 160
Brown solution F is incubated after 4h, Temperature fall to obtain at DEG C, in separatory funnel solution F is extracted with dichloromethane and it is static after, receive
Collection upper solution obtains brown viscous shape CQDs solution after being dialysed with bag filter；
4)CQDs/β-Bi2O3Preparation
Product D is transferred to after the CQDs solution stirring that 1ml is added in crucible, grinding, with water and washes of absolute alcohol, in
Freeze-day with constant temperature obtains CQDs/ β-Bi at 60 DEG C2O3Composite visible light catalyst.
Embodiment 4：
1)Bi2O2CO3Preparation
By 3mmol Bi (NO3)3·5H2O ultrasounds, which are dissolved in 15mL dilute nitric acid solution, is sufficiently stirred for obtaining solution A；
By 1mmol C6H8O7·H2O, which is added in solution A, is sufficiently stirred for obtaining settled solution B；
The pH value that 2mol/L NaOH solution to solution B is added dropwise into the solution B of clarification with microsyringe is 4.5；
Above-mentioned solution B is transferred in polytetrafluoroethylene (PTFE) water heating kettle, 24h is kept at 180 DEG C, with super after band reactor cooling
Pure water and absolute ethyl alcohol are respectively washed 3 times, and white product C i.e. Bi is obtained in drying at 80 DEG C2O2CO3；
2)β-Bi2O3Preparation
Take 1.0g products C to be uniformly layered in Noah's ark type corundum crucible, and be positioned over Muffle furnace, with 5 DEG C of heatings per minute
Speed is heated to 500 DEG C from room temperature, and keeps 2h, and it is β-Bi that product D is obtained after cooling2O3；
3) CQDs preparation
1g ascorbic acid is added to 15ml ethanol and water by 1:In the aqueous solution of the ethanol of 1 volume ratio mixing,
Settled solution E is obtained after ultrasound, solution E is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, at 160 DEG C
Be incubated 4h, after Temperature fall brown solution F, in separatory funnel solution F is extracted with dichloromethane and it is static after, in collection
Layer solution obtains brown viscous shape CQDs solution after being dialysed with bag filter；
4)CQDs/β-Bi2O3Preparation
Product D is transferred to after the CQDs solution stirring that 3ml is added in crucible, grinding, with water and washes of absolute alcohol, in
Freeze-day with constant temperature obtains CQDs/ β-Bi at 60 DEG C2O3Composite visible light catalyst.
Embodiment 5：
1)Bi2O2CO3Preparation
By 2.5mmol Bi (NO3)3·5H2O ultrasounds, which are dissolved in 20mL dilute nitric acid solution, is sufficiently stirred for obtaining solution A；
By 1.8mmol C6H8O7·H2O, which is added in solution A, is sufficiently stirred for obtaining settled solution B；
The pH value that 2mol/L NaOH solution to solution B is added dropwise into the solution B of clarification with microsyringe is 4.3；
Above-mentioned solution B is transferred in polytetrafluoroethylene (PTFE) water heating kettle, 24h is kept at 180 DEG C, with super after band reactor cooling
Pure water and absolute ethyl alcohol are respectively washed 3 times, and white product C i.e. Bi is obtained in drying at 80 DEG C2O2CO3；
2)β-Bi2O3Preparation
Take 1.0g products C to be uniformly layered in Noah's ark type corundum crucible, and be positioned over Muffle furnace, with 5 DEG C of heatings per minute
Speed is heated to 400 DEG C from room temperature, and keeps 2h, and it is β-Bi that product D is obtained after cooling2O3；
3) CQDs preparation
2.0g ascorbic acid is added to 30ml ethanol and water by 1:The aqueous solution of the ethanol of 1 volume ratio mixing
In, settled solution E is obtained after ultrasound, solution E is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, 160
Brown solution F is incubated after 4h, Temperature fall to obtain at DEG C, in separatory funnel solution F is extracted with dichloromethane and it is static after, receive
Collection upper solution obtains brown viscous shape CQDs solution after being dialysed with bag filter；
4)CQDs/β-Bi2O3Preparation
Product D is transferred to after the CQDs solution stirring that 4ml is added in crucible, grinding, with water and washes of absolute alcohol, in
Freeze-day with constant temperature obtains CQDs/ β-Bi at 60 DEG C2O3Composite visible light catalyst.
Claims (3)
1. a kind of CQDs/ β-Bi2O3Composite visible light catalyst, it is characterised in that：Shape is attached to by carbon quantum dot of uniform size
The irregular Bi of shape2O3Constituted in nanometer sheet.
2. a kind of CQDs/ β-Bi2O3The preparation method of composite visible light catalyst, it is characterised in that：
1)Bi2O2CO3Preparation
By 1~3mmol Bi (NO3)3·5H2O ultrasounds, which are dissolved in 5~20mL dilute nitric acid solution, is sufficiently stirred for obtaining solution A；
By 1~2mmol C6H8O7·H2O, which is added in solution A, is sufficiently stirred for obtaining settled solution B；
The pH value that 2mol/L NaOH solution to solution B is added dropwise into the solution B of clarification with microsyringe is 4.0~4.5；
Above-mentioned solution B is transferred in polytetrafluoroethylene (PTFE) water heating kettle, 24h is kept at 180 DEG C, ultra-pure water is used after band reactor cooling
It is respectively washed with absolute ethyl alcohol, white product C i.e. Bi is obtained in drying at 80 DEG C2O2CO3；
2)β-Bi2O3Preparation
Take 1.0g products C to be uniformly layered in Noah's ark type corundum crucible, and be positioned over Muffle furnace, with 5 DEG C of heating rates per minute
300~500 DEG C are heated to from room temperature, and keeps 2h, it is β-Bi that product D is obtained after cooling2O3；
3) CQDs preparation
In the aqueous solution that 0.5~2.0g ascorbic acid is added to 10~30ml ethanol, settled solution E is obtained after ultrasound,
Solution E is transferred in the stainless steel autoclave that polytetrafluoroethylene (PTFE) is liner, is incubated after 4h, Temperature fall and obtains at 160 DEG C
Brown solution F, with dichloromethane in separatory funnel to solution F extract and it is static after, collect upper solution dialysed with bag filter
Brown viscous shape CQDs solution is obtained afterwards；
4)CQDs/β-Bi2O3Preparation
Product D is transferred to after the CQDs solution stirring that 0.5ml, 1ml, 2ml, 3ml or 4ml are added in crucible, grinding, with water and
Washes of absolute alcohol, CQDs/ β-Bi are obtained in freeze-day with constant temperature at 60 DEG C2O3Composite visible light catalyst.
3. CQDs/ β-Bi according to claim 12O3The preparation method of composite visible light catalyst, it is characterised in that：Institute
The aqueous solution for the ethanol stated is ethanol and water by 1:The mixed solution of 1 volume ratio.
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