CN110354845A - A kind of bismuth tungstate photocatalyst and its preparation method and application of carbon nano dot modification - Google Patents
A kind of bismuth tungstate photocatalyst and its preparation method and application of carbon nano dot modification Download PDFInfo
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- CN110354845A CN110354845A CN201910576949.9A CN201910576949A CN110354845A CN 110354845 A CN110354845 A CN 110354845A CN 201910576949 A CN201910576949 A CN 201910576949A CN 110354845 A CN110354845 A CN 110354845A
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- bismuth
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- nano dot
- bismuth tungstate
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 85
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 82
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 82
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000002096 quantum dot Substances 0.000 title claims abstract description 77
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 51
- 230000004048 modification Effects 0.000 title claims abstract description 37
- 238000012986 modification Methods 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 58
- 239000002243 precursor Substances 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 34
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 18
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 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 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 11
- 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 abstract description 11
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 11
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 10
- QWMFKVNJIYNWII-UHFFFAOYSA-N 5-bromo-2-(2,5-dimethylpyrrol-1-yl)pyridine Chemical compound CC1=CC=C(C)N1C1=CC=C(Br)C=N1 QWMFKVNJIYNWII-UHFFFAOYSA-N 0.000 claims abstract description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000013049 sediment Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims description 13
- 238000002604 ultrasonography Methods 0.000 claims description 8
- 230000015556 catabolic process Effects 0.000 claims description 7
- 238000006731 degradation reaction Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 3
- 239000003344 environmental pollutant Substances 0.000 claims description 3
- 231100000719 pollutant Toxicity 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- BOATWIZKDIMFGZ-UHFFFAOYSA-N sodium nitrate pentahydrate Chemical compound O.O.O.O.O.[N+](=O)([O-])[O-].[Na+] BOATWIZKDIMFGZ-UHFFFAOYSA-N 0.000 claims description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- WZWGGYFEOBVNLA-UHFFFAOYSA-N sodium;dihydrate Chemical compound O.O.[Na] WZWGGYFEOBVNLA-UHFFFAOYSA-N 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 238000007254 oxidation reaction Methods 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 description 13
- 230000008859 change Effects 0.000 description 11
- 238000005245 sintering Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- -1 bismuth tungstate dihydrate Chemical class 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 5
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 3
- 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 3
- 230000004044 response Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 240000003273 Passiflora laurifolia Species 0.000 description 1
- 235000013762 Passiflora laurifolia Nutrition 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- B01J35/23—
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- 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
- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- 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 belongs to photocatalysis oxidation technique field, bismuth tungstate photocatalyst and its application of a kind of carbon nano dot modification are disclosed.The bismuth tungstate photocatalyst is to first pass through sodium tungstate dihydrate and deionized water preparation sodium tungstate precursor liquid A, and bismuth nitrate pentahydrate and dilute nitric acid solution prepare bismuth nitrate precursor liquid B；Precursor liquid A and B are blended in 100~250 DEG C of progress hydro-thermal reactions, after sediment is washed with deionized, calcined after dry at 400~520 DEG C, grind to obtain powder bismuth tungstate powder；Ethylenediamine solution and Citric Acid Mono are dissolved in the carbon nano dot precursor liquid of deionized water preparation in 100~300 DEG C of hydro-thermal reactions, the carbon nanodot solution being obtained by filtration, which is added drop-wise in bismuth tungstate powder, to be mixed, and dry, grinding is made.The bismuth tungstate photocatalyst of carbon nano dot modification has the ability of excellent photochemical catalytic oxidation organic pollutant, which can be used for the organic pollutants such as photochemical catalytic oxidation rhodamine B, phenol.
Description
Technical field
The invention belongs to photocatalysis oxidation technique fields, more particularly, to a kind of bismuth tungstate light of carbon nano dot modification
Catalyst and its preparation method and application.
Background technique
Problem of environmental pollution is one of Social Events of facing mankind, as human society is to organic chemicals
It is widely used, the discharge of organic industrial sewage, finding high performance, environmentally friendly ideal photochemical catalyst is scientific research
The target that field is struggled on without cease for it.Photocatalysis oxidation technique is a branch of emerging photocatalysis field, photocatalytic-oxidation
Change technology is using solar energy as energy source, using catalyst as a kind of green technology of medium degradable organic pollutant.
Photocatalytic oxidation degradation organic pollutant is even more ideal compared to traditional physical treatment, chemical degradation, microbial degradation etc..Light
The problem of catalytic oxidation technologies overriding concern is that the reasonable selection of photochemical catalyst, ideal photochemical catalyst should have photocatalytic
The excellent photoelectrochemical behaviours such as energy is good, chemical stability is good, visible light optical response range is wide, while relating to actual answer
With ideal photochemical catalyst also needs have the advantages such as preparation process is simple, low in cost, raw material amount of storage is big.
Bismuth tungstate is a kind of typical semiconductor light-catalyst, has suitable valence band and conduction band positions, forbidden bandwidth
Eg=2.7eV-2.8eV, can response section visible light, preparation process is simple, and physics, chemical stability are good, low in cost, is one
The more satisfactory semi-conducting ternary metal oxide photocatalyst of kind.But due to the higher photo-generated carrier of bismuth tungstate photocatalyst
Recombination rate, the less reaction site in surface make bismuth tungstate that the theoretical threshold values of photoelectric conversion much be not achieved.In order to make bismuth tungstate light
Catalyst obtains better photocatalysis performance, and the modification technology of many maturations is used for bismuth tungstate photocatalyst property modification, such as
Noble metal nano particles modification, doping, formation hetero-junctions, co-catalyst load etc..Herein, the present invention is come using carbon nano dot
Modify the bismuth tungstate photocatalyst of powder.
Carbon nano dot has extraordinary electric conductivity, and the photo-generated carrier that can be generated with fast transfer catalyst reduces light
The compound of carrier is given birth to, at the same time, the modification of carbon nano dot can further enhance photochemical catalyst and ring in the light of visible-range
Response and light absorpting ability, in addition, carbon nano dot cost is more low compared to dye nanoparticle and noble metal nano particles
It is honest and clean, chemical stability is more preferable, more friendly to environment, therefore, carbon nano dot is a kind of ideal co-catalysis material.This hair
The bright bismuth tungstate photocatalyst combination drying using carbon nanodot solution made from simple hydro-thermal method and powder, can obtain after grinding
Obtain the powder bismuth tungstate photocatalyst of carbon nano dot modification.Preparation process is very simple, is conducive to the popularization of practical application.
The bismuth tungstate photocatalyst of carbon nano dot modification is that the carbon nano dot of small particle is loaded by Van der Waals interaction
On bismuth tungstate photocatalyst surface, carbon nano dot functions similarly to the effect of active site.In the photocatalytic process, bismuth tungstate produces
Raw light induced electron is transferred on the carbon nano dot on bismuth tungstate surface by revolving speed, and participates in redox reaction, in solution
Organic pollutant is decomposed into avirulent small molecule or completely point oxygenolysis.Meanwhile carbon nano dot is since itself is very narrow
Forbidden bandwidth, most visible lights can be responded, its own also can produce photo-generate electron-hole to participate in react, further
The photocatalysis performance for promoting bismuth tungstate photocatalyst.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art, primary and foremost purpose of the present invention is to provide a kind of carbon nanometer
The bismuth tungstate photocatalyst of point modification.
Another object of the present invention is to provide the preparation methods of the bismuth tungstate photocatalyst of above-mentioned carbon nano dot modification.
A further object of the present invention is to provide the applications of the bismuth tungstate photocatalyst of above-mentioned carbon nano dot modification.
The purpose of the present invention is realized by following technical proposals:
A kind of bismuth tungstate photocatalyst of carbon nano dot modification, the bismuth tungstate photocatalyst is to first pass through sodium tungstate two
Hydrate and deionized water prepare sodium tungstate precursor liquid A, and bismuth nitrate pentahydrate and dilute nitric acid solution prepare bismuth nitrate precursor liquid
B；Precursor liquid A and B are blended in 100~250 DEG C of progress hydro-thermal reactions, after sediment is washed with deionized to precipitating
Solution is in neutrality afterwards, is calcined after dry at 400~520 DEG C, is ground to obtain powder bismuth tungstate powder；By ethylenediamine solution and a water lemon
The carbon nano dot precursor liquid that lemon acid dissolution is prepared in deionized water will filter after reaction in 100~300 DEG C of progress hydro-thermal reactions
To carbon nanodot solution be added drop-wise in bismuth tungstate powder and mix, dry, grinding is made.
Preferably, the sodium tungstate precursor liquid is that sodium tungstate dihydrate is dissolved in deionized water, ultrasonic to completely molten
Solution is made, wherein the volume ratio of the amount of the substance of the sodium tungstate dihydrate and deionized water is (1~5) mmol:10ml.
Preferably, the sodium nitrate precursor liquid is the dilute nitric acid solution that sodium nitrate pentahydrate is dissolved in pH value and is 3~6
In, ultrasound is obtained to being completely dissolved；Wherein, the amount of the substance of the bismuth nitrate pentahydrate and the volume ratio of dust technology be (1~
5) mmol:10ml.
Preferably, the volume ratio of the sodium tungstate precursor liquid and bismuth nitrate precursor liquid is (0.5~1.5): 1.
Preferably, the time that hydro-thermal reaction is carried out at 100~250 DEG C is 1~5h；It is described to be carried out at 100~300 DEG C
The time of hydro-thermal reaction is 3~20h.
Preferably, the time of the calcining is 1.5~4h；The temperature of the drying is 60~200 DEG C, and the dry time is
5~12h.
Preferably, the volume of the ethylenediamine solution: the quality of Citric Acid Mono: the volume ratio of deionized water be (0.1~
1) ml:(1~4) g:35ml.
Preferably, the mass ratio of the volume and bismuth tungstate powder of the carbon nanodot solution is (1~3) ml:3g.
The preparation method of the bismuth tungstate photocatalyst of the carbon nano dot modification, comprises the following specific steps that:
S1. sodium tungstate dihydrate and deionized water are prepared into sodium tungstate precursor liquid A, bismuth nitrate pentahydrate and dust technology
Solution prepares bismuth nitrate precursor liquid B；
S2. precursor liquid A and B are blended in 100~250 DEG C of progress hydro-thermal reactions, after by sediment deionized water
Washing solution to after precipitating is in neutrality, and is calcined after dry at 400~520 DEG C, is ground to obtain powder bismuth tungstate powder；
S3. by ethylenediamine solution and Citric Acid Mono be dissolved in the carbon nano dot precursor liquid of deionized water preparation 100~
The carbon nanodot solution being obtained by filtration, is added drop-wise in bismuth tungstate powder after reaction and mixes by 300 DEG C of progress hydro-thermal reactions, dry,
Grind the bismuth tungstate photocatalyst that the modification of carbon nano dot is made.
The bismuth tungstate photocatalyst of the carbon nano dot modification is in rhodamine B degradation or phenol organic chemical industry's pollutant
Application.
In the present invention carbon nano dot modify powder bismuth tungstate photocatalyst be mainly utilize carbon nano dot high conductivity,
The excellent photoelectric characteristics such as high photoproduction electron transfer capacity, high light absorpting ability to the photocatalysis performance of bismuth tungstate photocatalyst into
One step improves, and makes up the high photoproduction electron-hole pair recombination rate of bismuth tungstate conductor photocatalysis material, low electron transfer capacity and low
The performances such as visible light-responded.The powder bismuth tungstate photocatalyst of carbon nano dot modification has good light in visible light region
Absorbability, photo-generated carrier transfer ability, while the modification of carbon nano dot indirectly increases bismuth tungstate photocatalyst surface
Active site, the ability of the comprehensive photochemical catalytic oxidation organic pollutant for improving bismuth tungstate photocatalyst, which can
For organic pollutants such as photochemical catalytic oxidation rhodamine B, phenol.
Compared with prior art, the invention has the following advantages:
1. the bismuth tungstate photocatalyst that carbon nano dot of the invention is modified has widened pure tungsten acid due to the modification of carbon nano dot
Visible light optical responsivity and light absorpting ability of the bismuth photochemical catalyst in 380nm-780nm wave-length coverage.
It, can fast transfer bismuth tungstate photocatalyst 2. carbon nano dot is carried on bismuth tungstate photocatalyst surface in the present invention
Photo-generated carrier, inhibits the compound of photo-generate electron-hole pair, and carbon nano dot plays the role of similar active site.
3. the carbon nano dot and bismuth tungstate in the present invention all have environmentally friendly, chemical stabilization, low in cost, preparation work
The advantages that skill is simple is conducive to the popularization of practical application.
4. the bismuth tungstate photocatalyst that carbon nano dot is modified in the present invention can be used for rhodamine B degradation, phenol etc. and organise
Work pollutant, broadly, it is that other similar semiconductor light-catalyst photocatalysis performance modification mentions that carbon nano dot, which can be modified,
It is referred to and learnt from for strategy.
Detailed description of the invention
Fig. 1 is the ultraviolet of the powder bismuth tungstate photocatalyst rhodamine B degradation of the carbon nano dot modification prepared in embodiment 1
Visible absorbance map.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Embodiment 1
1. 1.5mmol bismuth tungstate dihydrate is taken to be dissolved in the deionized water of 10ml, tungsten is made to being completely dissolved in ultrasound
Sour sodium precursor liquid.
2. take 1.5mmol bismuth nitrate pentahydrate to be dissolved in the dilute nitric acid solution of the pH=6 of 10ml, it is ultrasonic to completely molten
Bismuth nitrate precursor liquid is made in solution.
3.10ml sodium tungstate precursor liquid is mixed with 10ml bismuth nitrate precursor liquid, obtains milky bismuth tungstate precursor liquid, is turned
It moves in the pyroreaction kettle of 50ml, hydro-thermal reaction 2h at a temperature of 120 DEG C.After hydro-thermal, deposit uses deionized water
Washing 5 times, the deposit after washing is placed in silica dish, is transferred to Muffle furnace, under air atmosphere, 450 DEG C of sintering 2h.It burns
After knot, grinding obtains the bismuth tungstate powder of powder.
4. carbon nanodot solution is prepared by simple hydro-thermal reaction, carbon nano dot precursor liquid is by ethylenediamine solution: a water
Citric acid: deionized water=0.2ml:2g:35ml is mixed under stirring conditions, is transferred to the pyroreaction kettle of 50ml
In, hydro-thermal reaction 3h under the conditions of 150 DEG C is filtered using bag filter, and carbon nanodot solution is made.
5. 1ml carbon nanodot solution is taken to be uniformly mixed with 2g bismuth tungstate powder, brown pureed is transferred to vacuum drying
Case, under vacuum conditions, dry 8h, grinding at a temperature of 150 DEG C obtain the nano-modified bismuth tungstate photocatalyst of carbon.
Take carbon nano dot made from 0.03g modify bismuth tungstate photocatalyst under the conditions of magnetic agitation, simulated solar irradiation
The rhodamine B solution that irradiation degradation 10ml concentration is 10mg/L is modified with tinfoil package added with carbon nano dot before illumination degrading
Powder bismuth tungstate photocatalyst rhodamine B solution magnetic agitation for 24 hours, allow rhodamine B molecule to be sufficiently adsorbed on photochemical catalyst
On surface.
Fig. 1 is the purple that the bismuth tungstate photocatalyst of the modification of carbon nano dot made from the present embodiment degrades to rhodamine B solution
Outer visible absorbance analyzes spectrum, from figure 1 it appears that the bismuth tungstate photocatalyst after the modification of carbon nano dot will be molten in 6min
Rhodamine B of the solution in deionized water is degraded to rapidly very low concentration, almost degrades after 20min.
Embodiment 2
1. 5mmol bismuth tungstate dihydrate is taken to be dissolved in the deionized water of 10ml, wolframic acid is made to being completely dissolved in ultrasound
Sodium precursor liquid.
2. 1mmol bismuth nitrate pentahydrate is taken to be dissolved in the dilute nitric acid solution of the pH=6 of 10ml, ultrasound to being completely dissolved,
Bismuth nitrate precursor liquid is made.
3.5ml sodium tungstate precursor liquid is mixed with 10ml bismuth nitrate precursor liquid, obtains milky bismuth tungstate precursor liquid, transfer
Into the pyroreaction kettle of 50ml, hydro-thermal reaction 5h at a temperature of 100 DEG C.After hydro-thermal, deposit makes to be washed with deionized water
It washs 5 times, the deposit after washing is placed in silica dish, it is transferred to Muffle furnace, under air atmosphere, 400 DEG C of sintering 4h.Sintering
After, grinding obtains the bismuth tungstate powder of powder.
4. carbon nanodot solution is prepared by simple hydro-thermal reaction, carbon nano dot precursor liquid is by ethylenediamine solution: a water
Citric acid: deionized water=0.2ml:2g:35ml is mixed under stirring conditions, is transferred to the pyroreaction kettle of 50ml
In, hydro-thermal reaction 10h under the conditions of 100 DEG C is filtered using bag filter, and carbon nanodot solution is made.
5. 1ml carbon nanodot solution is taken to be uniformly mixed with 3g bismuth tungstate powder, brown pureed is transferred to vacuum drying
Case, under vacuum conditions, dry 5h, grinding at a temperature of 200 DEG C obtain the nano-modified bismuth tungstate photocatalyst of carbon.
Embodiment 3
1. 1.mmol bismuth tungstate dihydrate is taken to be dissolved in the deionized water of 10ml, tungsten is made to being completely dissolved in ultrasound
Sour sodium precursor liquid.
2. 5mmol bismuth nitrate pentahydrate is taken to be dissolved in the dilute nitric acid solution of the pH=5 of 10ml, ultrasound to being completely dissolved,
Bismuth nitrate precursor liquid is made.
3.10ml sodium tungstate precursor liquid is mixed with 5ml bismuth nitrate precursor liquid, obtains milky bismuth tungstate precursor liquid, transfer
Into the pyroreaction kettle of 50ml, hydro-thermal reaction 1h at a temperature of 250 DEG C.After hydro-thermal, deposit makes to be washed with deionized water
It washs 5 times, the deposit after washing is placed in silica dish, it is transferred to Muffle furnace, under air atmosphere, 520 DEG C of sintering 1.5h.It burns
After knot, grinding obtains the bismuth tungstate powder of powder.
4. carbon nanodot solution is prepared by simple hydro-thermal reaction, carbon nano dot precursor liquid is by ethylenediamine solution: a water
Citric acid: deionized water=0.2ml:2g:35ml is mixed under stirring conditions, is transferred to the pyroreaction kettle of 50ml
In, hydro-thermal reaction 3h under the conditions of 300 DEG C is filtered using bag filter, and carbon nanodot solution is made.
5. 2ml carbon nanodot solution is taken to be uniformly mixed with 2g bismuth tungstate powder, brown pureed is transferred to vacuum drying
Case, under vacuum conditions, dry 12h, grinding at a temperature of 60 DEG C obtain the nano-modified bismuth tungstate photocatalyst of carbon.
Embodiment 4
The present embodiment the difference from embodiment 1 is that, configure sodium tungstate precursor liquid when, the substance of sodium tungstate dihydrate
Amount is incremental change by 1mmol, configures the sodium tungstate precursor liquid of various concentration within the scope of 1-5mmol.
Embodiment 5
The present embodiment the difference from embodiment 1 is that, configure bismuth nitrate precursor liquid when, the substance of bismuth nitrate pentahydrate
Amount is incremental change by 1mmol, configures the bismuth tungstate precursor liquid of various concentration in the range of 1-5mml.
Embodiment 6
The present embodiment the difference from embodiment 1 is that, configure bismuth nitrate precursor liquid when, dilute nitric acid solution pH value be 3-5
In the range of, by the incremental gradient of pH=0.5, the dilute nitric acid solution of different pH value is configured, for configuring bismuth nitrate precursor liquid.
Embodiment 7
The present embodiment the difference from embodiment 1 is that, bismuth tungstate precursor liquid hydrothermal temperature be 100-250 DEG C within the scope of,
With 30 DEG C of increasing temperature, carry out hydro-thermal reaction at different temperatures.
Embodiment 8
The present embodiment the difference from embodiment 1 is that, the bismuth tungstate precursor liquid hydro-thermal time is with 1h in the range of 1-5h
Incremental change controls the time of hydro-thermal reaction.
Embodiment 9
The present embodiment the difference from embodiment 1 is that, sintering temperature is within the scope of 400-520 DEG C, with 20 DEG C for incremental change,
Obtain the bismuth tungstate powder under different sintering temperatures.
Embodiment 10
The present embodiment the difference from embodiment 1 is that, sintering time is in the range of 1.5-4h, using 30min as incremental change,
Obtain the sample of different soaking times.
Embodiment 11
The present embodiment the difference from embodiment 1 is that, carbon nano dot precursor liquid hydrothermal temperature within the scope of 100-300 DEG C,
With 50 DEG C for incremental change, the carbon nano-solution under different hydrothermal temperatures is obtained.
Embodiment 12
The present embodiment the difference from embodiment 1 is that, the carbon nano dot precursor liquid hydro-thermal time within the scope of 3-20h, with 2h
For incremental change, the carbon nanodot solution of different soaking times is obtained.
Embodiment 13
The present embodiment the difference from embodiment 1 is that, vacuum drying temperature is in 60-200 DEG C of temperature range, with 20 DEG C
Incremental change obtains the sample under different temperatures.
Embodiment 14
The present embodiment the difference from embodiment 1 is that, the vacuum drying time within the scope of 5-12h, using 2h as incremental change,
Obtain the sample of different drying times.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of bismuth tungstate photocatalyst of carbon nano dot modification, which is characterized in that the bismuth tungstate photocatalyst is first logical
Pertungstic acid sodium dihydrate and deionized water prepare sodium tungstate precursor liquid A, and bismuth nitrate pentahydrate and dilute nitric acid solution prepare nitre
Sour bismuth precursor liquid B；Precursor liquid A and B are blended in 100~250 DEG C of progress hydro-thermal reactions, after by sediment deionized water
Washing solution to after precipitating is in neutrality, and is calcined after dry at 400~520 DEG C, is ground to obtain powder bismuth tungstate powder；Ethylenediamine is molten
Liquid and Citric Acid Mono are dissolved in the carbon nano dot precursor liquid of deionized water preparation in 100~300 DEG C of progress hydro-thermal reactions, reaction
The carbon nanodot solution being obtained by filtration is added drop-wise in bismuth tungstate powder afterwards and is mixed, dry, grinding is made.
2. the bismuth tungstate photocatalyst of carbon nano dot modification according to claim 1, which is characterized in that before the sodium tungstate
Driving liquid is that sodium tungstate dihydrate is dissolved in deionized water, and ultrasound is obtained to being completely dissolved, wherein the sodium tungstate two is hydrated
The amount of the substance of object and the volume ratio of deionized water are (1~5) mmol:10ml.
3. the bismuth tungstate photocatalyst of carbon nano dot modification according to claim 1, which is characterized in that before the sodium nitrate
Driving liquid is in the dilute nitric acid solution that sodium nitrate pentahydrate is dissolved in pH value and is 3~6, and ultrasound is obtained to being completely dissolved；Wherein,
The amount of the substance of the bismuth nitrate pentahydrate and the volume ratio of dust technology are (1~5) mmol:10ml.
4. the bismuth tungstate photocatalyst of carbon nano dot modification according to claim 1, which is characterized in that before the sodium tungstate
The volume ratio for driving liquid and bismuth nitrate precursor liquid is (0.5~1.5): 1.
5. the bismuth tungstate photocatalyst of carbon nano dot according to claim 1 modification, which is characterized in that it is described 100~
The time of 250 DEG C of progress hydro-thermal reactions is 1~5h；The time that hydro-thermal reaction is carried out at 100~300 DEG C is 3~20h.
6. the bismuth tungstate photocatalyst of carbon nano dot according to claim 1 modification, which is characterized in that the calcining when
Between be 1.5~4h；The temperature of the drying is 60~200 DEG C, and the dry time is 5~12h.
7. the bismuth tungstate photocatalyst of carbon nano dot modification according to claim 1, which is characterized in that the ethylenediamine is molten
The volume of liquid: the quality of Citric Acid Mono: the volume ratio of deionized water is (0.1~1) ml:(1~4) g:35ml.
8. the bismuth tungstate photocatalyst of carbon nano dot modification according to claim 1, which is characterized in that the carbon nano dot
The volume of solution and the mass ratio of bismuth tungstate powder are (1~3) ml:3g.
9. the preparation method of the bismuth tungstate photocatalyst of carbon nano dot modification according to claim 1-8, special
Sign is, comprises the following specific steps that:
S1. sodium tungstate dihydrate and deionized water are prepared into sodium tungstate precursor liquid A, bismuth nitrate pentahydrate and dilute nitric acid solution
Prepare bismuth nitrate precursor liquid B；
S2. precursor liquid A and B are blended in 100~250 DEG C of progress hydro-thermal reactions, after sediment is washed with deionized
Solution is in neutrality after to precipitating, is calcined after dry at 400~520 DEG C, is ground to obtain powder bismuth tungstate powder；
S3. ethylenediamine solution and Citric Acid Mono are dissolved in the carbon nano dot precursor liquid of deionized water preparation at 100~300 DEG C
Hydro-thermal reaction is carried out, the carbon nanodot solution being obtained by filtration is added drop-wise in bismuth tungstate powder after reaction and is mixed, dry, grinding system
Obtain the bismuth tungstate photocatalyst of carbon nano dot modification.
10. the bismuth tungstate photocatalyst of the described in any item carbon nano dot modifications of claim 1-8 is in rhodamine B degradation or phenol
Application in organic chemical industry's pollutant.
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