CN105597764B - A kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material - Google Patents
A kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material Download PDFInfo
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- CN105597764B CN105597764B CN201610132912.3A CN201610132912A CN105597764B CN 105597764 B CN105597764 B CN 105597764B CN 201610132912 A CN201610132912 A CN 201610132912A CN 105597764 B CN105597764 B CN 105597764B
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- zinc ferrite
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 229910001308 Zinc ferrite Inorganic materials 0.000 title claims abstract description 98
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 59
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 42
- 239000007864 aqueous solution Substances 0.000 claims abstract description 35
- 239000008367 deionised water Substances 0.000 claims abstract description 26
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 26
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000000725 suspension Substances 0.000 claims abstract description 21
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 20
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 20
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 150000003751 zinc Chemical class 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 22
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 16
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical group [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 8
- 239000011592 zinc chloride Substances 0.000 claims description 8
- 235000005074 zinc chloride Nutrition 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 description 16
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 16
- 230000001699 photocatalysis Effects 0.000 description 11
- 235000011121 sodium hydroxide Nutrition 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 238000001035 drying Methods 0.000 description 9
- 238000007146 photocatalysis Methods 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000011701 zinc Substances 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000007900 aqueous suspension Substances 0.000 description 5
- 230000006798 recombination Effects 0.000 description 5
- 238000005215 recombination Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910000161 silver phosphate Inorganic materials 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 150000008107 benzenesulfonic acids Chemical class 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940106691 bisphenol a Drugs 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- RDUJRVXKAIVTDH-UHFFFAOYSA-N chembl2008747 Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C(S(O)(=O)=O)C=C1 RDUJRVXKAIVTDH-UHFFFAOYSA-N 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- RLBIQVVOMOPOHC-UHFFFAOYSA-N parathion-methyl Chemical group COP(=S)(OC)OC1=CC=C([N+]([O-])=O)C=C1 RLBIQVVOMOPOHC-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)
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Abstract
A kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material, ascorbic acid is added in ethylene glycol and the mixed solution of deionized water, reacts 1 5h after stirring at 100 200 DEG C, obtains the carbon quantum dot aqueous solution；By zinc salt and Fe (NO3)3·9H2O is added to the water, and it is 8 14 that pH value is adjusted after dissolving, obtains suspension；The carbon quantum dot aqueous solution is added in suspension, stood after stirring, then the 10h of hydro-thermal reaction 4 at 80 180 DEG C, is washed out, dries, and obtains carbon quantum dot/zinc ferrite composite photocatalyst material.The raw material of the present invention is cheap to be easy to get, synthesizes that cost is relatively low, method is simple and easy, carbon quantum dot/zinc ferrite compared to pure zinc ferrite in visible-range to NOxWith higher degradation efficiency.
Description
Technical field
A kind of photocatalysis technology field of the present invention, and in particular to the preparation of carbon quantum dot/zinc ferrite composite photocatalyst material
Method.
Background technology
Nitrogen oxides (NOx) as common air pollutants, including NO and NO2, it is to produce greenhouse effects, acid rain, ozone
Cavity, photochemical fog and PM2.5One of major pollutants, also can be directly or indirectly to the mankind to the very harmful of environment
Health damages.Gas denitrifying technology mainly industrially is used at present, so as to reach NOxCan discharge standard.But NOxConcentration
It is relatively low in atmosphere, can not effectively it be removed with traditional method.The nitrogen oxides accumulated in long-term air in the past can influence
To the air quality of human habitat, therefore there is an urgent need to effectively handle the pollutant.Research is found：Photocatalytic redox
The characteristics of reaction is had rapidly and efficiently in the application of degradation of contaminant, and required equipment is simple, good product selectivity, reaction
Mild condition etc., therefore the technology has broad application prospects in terms of environment pollution control.
The ZnFe of spinel structure2O4It is the narrower semiconductor of a kind of band gap (~2.0eV), to visible in solar spectrum
Light has response, and raw material storage is abundant, cheap, nontoxic and environmentally friendly.But the recombination rate in its light induced electron and hole
It is too fast, so as to reduce its photocatalytic activity, it is therefore desirable to which finding a kind of effective method reduces its light induced electron and hole
Recombination rate.Patent CN103887081A uses Hydrothermal Synthesiss nitrogen-doped graphene/zinc ferrite nano composite material, zinc ferrite to exist
The surface of nitrogen-doped graphene, prevent the accumulation of nitrogen-doped graphene between layers to reunite, improve its electrochemical properties.
Patent CN104437573A is prepared for ZnFe using ion exchange technique2O4/Ag3PO4Composite photo-catalyst, it is heterogeneous by building
Knot body system realizes the high efficiente callback of photochemical catalyst, and ZnFe2O4/Ag3PO4Drop of the composite photo-catalyst to antibiotic in waste water
It is better than pure zinc ferrite and silver orthophosphate to solve effect；Patent CN104437574A with carbosphere (CMSs) for core, using solvent-thermal method
With in situ Precipitation by zinc ferrite (ZnFe2O4), silver orthophosphate (Ag3PO4) carbosphere surface is supported on successively, it is made with anti-light
Corrosive double-deck core shell structure composite catalyst MSs ZnFe2O4@Ag3PO4；Patent CN104383930A uses microwave hydrothermal
Zinc ferrite load carbon nano-tube catalyst prepared by method, the catalyst and five kinds of organic pollutions (ten in microwave combined degradation water
Dialkyl benzene sulfonic acids sodium, Acid Orange II, methyl orange, parathion-methyl and bisphenol-A) speed, degradation efficiency it is high, without in
Between product generate, secondary pollution will not be caused；It is multiple that patent CN104941671A by the precipitation method has synthesized zinc ferrite/bismuth oxyiodide
Visible light catalyst is closed, 90% is up to the degradation rate of methyl orange dye waste water under natural light.
Carbon quantum dot (Carbon Quantum Dots, CQDs) is a kind of new carbon nanomaterial, size 10nm with
Under, there is good water solubility, hypotoxicity, be easy to the excellent properties such as functionalization and anti-light stability.In addition, luminescence generated by light
The wavelength excited further increases its photocatalysis performance.Therefore, carbon quantum dot (CQDs) has in terms of photocatalysis technology and lured
The prospect of people.Patent CN103480353A makees mixed solvent by carbon source, water and ethanol of vitamin C, passes through hydrothermal synthesis of carbon
Quantum dot, titanium dioxide powder and carbon quantum dot solution mixing system are obtained into composite photo-catalyst, the composite is to methylene blue
Degradation rate it is higher；Multi-functional meso-porous titanium dioxide of the patent CN104877677A synthesis with ordered mesopore structure and fluorescence property
Silicon/carbon quantum dot nano composite material；In the prior art by preparing methyl in the degradation waste water containing carbon quantum dot
Orange, methylene blue etc., but nitrogen oxides can not be degraded.
Research shows：Carbon quantum dot (CQDs) can be used as electronic storage, receive the light induced electron of semiconductor catalyst,
So as to reduce semiconductor (SiO2、TiO2、ZnO、Fe2O3、Cu2O、Ag3PO4Deng) light induced electron and hole recombination rate.Simultaneously
Carbon quantum dot has up conversion property, can absorb the longer part of sunshine medium wavelength, launches shortwave (325-425nm), enters
And exciting the larger semiconductor light-catalyst of energy gap to form electron hole pair, electron hole pair again can be with the oxidant of absorption
Reacted with reducing agent and produce active oxygen radical, so as to degradation of contaminant.
The content of the invention
It is an object of the invention to provide a kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material, this method
The composite photocatalyst material of preparation can be to NO in visible-rangexPhotocatalytic degradation, and synthetic method is simple, raw material is low
It is honest and clean to be easy to get.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material, comprises the following steps：
A. ascorbic acid is added in ethylene glycol and the mixed solution of deionized water, at 100-200 DEG C after stirring
Lower reaction 1-5h, obtains the carbon quantum dot aqueous solution；Wherein, ascorbic acid, ethylene glycol, the ratio of deionized water are (0.5-5.0) g：
(5.0-30)mL：(10-50)mL；
B. by zinc salt and Fe (NO3)3·9H2O is added to the water, and it is 8-14 that pH value is adjusted after dissolving, obtains suspension；Its
In, zinc salt and Fe (NO3)3·9H2O mol ratio is 1：(0.1-5.0), Fe (NO3)3·9H2The ratio of O and water is (1.0-5.0)
g：(10-50)mL；
C. the carbon quantum dot aqueous solution is added in suspension, stood after stirring, then the hydro-thermal at 80-180 DEG C
4-10h is reacted, is washed out, dries, obtain carbon quantum dot/zinc ferrite composite photocatalyst material；Wherein, the carbon quantum dot aqueous solution
Volume ratio with suspension is (0.1-25) mL：(10-50)mL.
Zinc salt is zinc nitrate, zinc chloride or zinc acetate in the step b.
Using sodium hydroxide solution or ammonia spirit regulation pH value in the step b.
The sodium hydroxide solution, the concentration of ammoniacal liquor are 2mol/L.
The time stood in the step c is 1 day.
Washed in the step c and be specially：Deionized water and ethanol washing is respectively adopted.
The temperature dried in the step c is 50-100 DEG C.
Compared with prior art, the device have the advantages that：
The present invention is closed using low cost feedstocks such as ascorbic acid, zinc nitrate, ferric nitrate, sodium hydroxides by simple hydro-thermal method
Into carbon quantum dot/zinc ferrite composite photo-catalyst, the raw material of the composite photo-catalyst is cheap to be easy to get, the relatively low, method that synthesizes cost
It is simple and easy, carbon quantum dot/zinc ferrite compared to pure zinc ferrite in visible-range to NOxImitated with higher degraded
Rate.The structure of carbon quantum dot prepared by the present invention/zinc ferrite composite photo-catalyst is identical with pure zinc ferrite, is all spinelle knot
Structure；In carbon quantum dot/zinc ferrite composite photo-catalyst zinc ferrite be average particle size be 10nm spherical nanoparticle, carbon amounts
Son point is distributed in the surface of zinc ferrite；When the dosage of the carbon quantum dot aqueous solution is 3mL, carbon quantum dot/zinc ferrite complex light is urged
Agent reaches highest to NO clearances, it is seen that light illumination 30min, NO clearance is up to 38%, and compared to pure zinc ferrite, (NO is removed
Rate is only 29%) to improve 9%.NO during the entire process of visible ray illumination 30min2Growing amount there is negative value, illustrate carbon amounts
Sub- point/zinc ferrite composite photo-catalyst can also degrade part NO2.When catalyst recycles six times, NO clearance does not have
The phenomenon of reduction is occurred, illustrates that the stability of composite photo-catalyst is higher, can be recycled for multiple times.Due to the forbidden band of zinc ferrite
Narrower width (~2.0eV), it is seen that photohole electronics pair can be produced under light, but its recombination rate is high, therefore photocatalysis performance
Relatively low, after carbon quantum dot and compound zinc ferrite, the light induced electron of zinc ferrite is transferred to carbon quantum dot, reduces the photoproduction of zinc ferrite
Electronics and the recombination rate in hole, and then improve the photocatalysis performance of zinc ferrite, therefore, compared to pure zinc ferrite, carbon quantum dot/
Zinc ferrite composite photo-catalyst is to NOxDegradation rate increase.
The present invention not only increases its utilization rate to solar energy by carbon quantum dot and the compound of zinc ferrite, and improves
The photocatalysis stability of zinc ferrite, the research have far reaching significance to the practical of photocatalysis technology.
Brief description of the drawings
Fig. 1 is the XRD spectra of pure zinc ferrite and carbon quantum dot/zinc ferrite composite photo-catalyst；
Fig. 2 is pure zinc ferrite and carbon quantum dot/zinc ferrite composite photo-catalyst NO under visible light the clearance time
Figure；
Fig. 3 is pure zinc ferrite and carbon quantum dot/zinc ferrite composite photo-catalyst NO under visible light2The growing amount time
Figure；
Fig. 4 is CQDs/ZnFe2O4The TEM figures of -2 composite photo-catalysts；
Fig. 5 is CQDs/ZnFe2O4- 2 composite photo-catalysts are degraded NO recycling performance figure under visible light.
Embodiment
Make specific introduce to the present invention below in conjunction with the drawings and specific embodiments.
Embodiment 1
A. 1.6g ascorbic acid is weighed, is added in 15mL ethylene glycol and the mixed solution of 25mL deionized waters, room temperature is stirred
30min is mixed, then reacts 70min at 160 DEG C, obtains the carbon quantum dot aqueous solution；
B. 1.189g Zn (NO are weighed respectively3)2·6H2O and 3.232g Fe (NO3)3·9H2O, then add 20mL and go
Ionized water, stir to solution and clarify at room temperature；
C. the pH value of 2mol/L NaOH solution regulating step b resulting solutions is used, pH value is reached 13.0, is suspended
Liquid；
D. the carbon quantum dot aqueous solution obtained by 1mL steps a is added into suspension obtained by above-mentioned steps c；
E. 1 day is stood after stirring, is then transferred into 100mL polytetrafluoroethylliner liner, hydro-thermal reaction at 100 DEG C
6h, then washed repeatedly with deionized water and ethanol respectively, 70 DEG C of drying, obtain carbon quantum dot/zinc ferrite composite photocatalyst material.
Embodiment 2
A. 1.6g ascorbic acid is weighed, is added in 15mL ethylene glycol and the mixed solution of 25mL deionized waters, room temperature is stirred
30min is mixed, then reacts 70min at 160 DEG C, obtains the carbon quantum dot aqueous solution；
B. 1.189g Zn (NO are weighed respectively3)2·6H2O and 3.232g Fe (NO3)3·9H2O, then add 20mL and go
Ionized water, stir to solution and clarify at room temperature；
C. the pH value of 2mol/L NaOH solution regulating step b resulting solutions is used, pH value is reached 13.0, is suspended
Liquid；
D. the carbon quantum dot aqueous solution obtained by 3mL steps a is added into suspension obtained by above-mentioned steps c；
E. 1 day is stood after stirring is well mixed for a period of time, is then transferred into 100mL polytetrafluoroethylliner liner, 100
Hydro-thermal reaction 6h at DEG C, then washed repeatedly with deionized water and ethanol respectively, 70 DEG C of drying, it is multiple to obtain carbon quantum dot/zinc ferrite
Closing light catalysis material.
Embodiment 3
A. 1.6g ascorbic acid is weighed, is added in the mixed solution of 15mL ethylene glycol and 25mL deionized waters, room temperature is stirred
30min is mixed, then reacts 70min at 160 DEG C, obtains the carbon quantum dot aqueous solution；
B. 1.189g Zn (NO are weighed respectively3)2·6H2O and 3.232g Fe (NO3)3·9H2O, then add 20mL and go
Ionized water, stir to solution and clarify at room temperature；
C. the pH value of 2mol/L NaOH solution regulating step b resulting solutions is used, pH value is reached 13.0, is suspended
Liquid；
D. the carbon quantum dot aqueous solution obtained by 5mL steps a is added into suspension obtained by above-mentioned steps c；
E. stirring a period of time to stand 1 day after being well mixed, and is then transferred into 100mL polytetrafluoroethylliner liner
In, hydro-thermal reaction 6h at 100 DEG C, then washed repeatedly with deionized water and ethanol respectively, 70 DEG C of drying, obtain carbon quantum dot/iron
Sour zinc composite photocatalyst material.
Embodiment 4
A. 1.6g ascorbic acid is weighed, is added in 15mL ethylene glycol and the mixed solution of 25mL deionized waters, room temperature is stirred
30min is mixed, then reacts 70min at 160 DEG C, obtains the carbon quantum dot aqueous solution；
B. 1.189g Zn (NO are weighed respectively3)2·6H2O and 3.232g Fe (NO3)3·9H2O, then add 20mL and go
Ionized water, stir to solution and clarify at room temperature；
C. the pH value of 2mol/L NaOH solution regulating step b resulting solutions is used, pH value is reached 13.0, is suspended
Liquid；
D. the carbon quantum dot aqueous solution obtained by 10mL steps a is added into suspension obtained by above-mentioned steps c；
E. stirring a period of time to stand 1 day after being well mixed, and is then transferred into 100mL polytetrafluoroethylliner liner
In, 6h is reacted at 100 DEG C, is washed repeatedly with deionized water and ethanol respectively, 70 DEG C of drying, it is multiple to obtain carbon quantum dot/zinc ferrite
Closing light catalysis material.
Carry out XRD tests respectively to pure zinc ferrite and carbon quantum dot/zinc ferrite composite photo-catalyst, test collection of illustrative plates is as schemed
Shown in 1.
As can be seen from Figure 1：Carbon quantum dot/zinc ferrite obtained by embodiment 1, embodiment 2, embodiment 3, embodiment 4
Composite photo-catalyst (i.e. CQDs/ZnFe2O4-1、CQDs/ZnFe2O4-2、CQDs/ZnFe2O4- 3 and CQDs/ZnFe2O4- 4) own
Diffraction maximum coincide with database JCPDS card No.22-1012 diffraction maximums, belong to spinel structure, show in carbon quantum dot
In the presence of having no effect on ZnFe2O4Structure, due to the comparision contents of carbon quantum dot in carbon quantum dot/zinc ferrite composite photo-catalyst
It is low, therefore there is no its characteristic peak in XRD spectra；
Visible light photocatalysis active survey is carried out respectively to pure zinc ferrite and carbon quantum dot/zinc ferrite composite photo-catalyst
Examination：
Photocatalytic degradation experiment is carried out in continuous flow reactor by target contaminant of NO.Using 300W xenon lamp as photograph
Light source is penetrated, wavelength X ＜ 400nm light is filtered by optical filter.Culture dish comprising 0.1g catalyst fines samples is placed
In the continuous flow reactor with quartz glass window, the NO that initial concentration is 400ppb is passed through.After steady air current, beat
Open xenon lamp test.Pass through the NO concentration in NO optical analysers (U.S.'s thermoelectricity, model 42c) dynamic monitoring reactor.With NO
The ratio and NO of exit concentration and initial concentration2Growing amount evaluate the catalytic performance of photochemical catalyst.
Fig. 2 is clearance time diagram of pure zinc ferrite and carbon quantum dot/the zinc ferrite composite photo-catalyst to NO.By Fig. 2
As can be seen that prepared carbon quantum dot/zinc ferrite composite photo-catalyst shows preferable degradation property to NO.Work as carbon quantum
When the dosage of the point aqueous solution is less than 3mL, with the increase of carbon quantum dot amount of aqueous solution used, NO clearances also gradually increase；Afterwards
When gradually increasing the dosage of the carbon quantum dot aqueous solution again, there have been the trend of reduction for NO clearances；Therefore, when carbon quantum dot water
When the dosage of solution is 3mL, carbon quantum dot/zinc ferrite composite photo-catalyst reaches highest to NO clearances, it is seen that light illumination
30min, NO clearance improve 9% up to 38%, compared to pure zinc ferrite (NO clearances are only 29%).
Fig. 3 is the process NO that pure zinc ferrite and carbon quantum dot/zinc ferrite composite photo-catalyst remove NO2Growing amount-
Time diagram.When photochemical catalyst is carbon quantum dot/zinc ferrite composite photo-catalyst, NO2Growing amount compared to pure zinc ferrite come
Say relatively low, it is seen that NO during the entire process of light illumination 30min2Growing amount there is negative value, illustrate that carbon quantum dot/zinc ferrite is compound
Photochemical catalyst can also degrade part NO2。
To CQDs/ZnFe2O4- 2 carry out TEM tests, and test collection of illustrative plates is as shown in Figure 3.
From fig. 4, it can be seen that the CQDs/ZnFe obtained by embodiment 22O4In the TEM spectrograms of -2 composite photo-catalysts
0.25nm and 0.29nm lattice fringe corresponds to ZnFe respectively2O4(311) and (200) crystal face, 0.32nm lattice fringe is corresponding
(002) crystal face of carbon quantum dot, zinc ferrite are spheric granules, and average ion size is 10nm, and carbon quantum dot is distributed in iron
The surface of sour zinc.
Fig. 5 is CQDs/ZnFe2O4- 2 composite photo-catalysts are degraded NO recycling performance figure under visible light.CQDs/
ZnFe2O4- 2 have higher degradation efficiency to NO under visible light, and when catalyst recycles six times, NO clearance does not have
The phenomenon of reduction is occurred, illustrates CQDs/ZnFe2O4The stability of -2 composite photo-catalysts is higher, can be recycled for multiple times.
As can be seen here, the present invention can be prepared by the carbon quantum with compared with high visible light catalytic activity by simple hydro-thermal method
Point/zinc ferrite composite photo-catalyst, not only preparation process is simple to operation, and raw material it is cheap be easy to get it is nontoxic.
Because the carbon quantum dot in carbon quantum dot/zinc ferrite composite photo-catalyst can store part electronics, be advantageous to iron
The light induced electron of sour zinc and efficiently separating for photohole, the light of long wavelength can also be absorbed and then inspire the light of short wavelength,
Make carbon quantum dot/zinc ferrite composite photo-catalyst that there is more preferable photocatalysis performance than pure zinc ferrite.
Embodiment 5
A. ascorbic acid is added in ethylene glycol and the mixed solution of deionized water, it is anti-at 100 DEG C after stirring
5h is answered, obtains the carbon quantum dot aqueous solution；Wherein, ascorbic acid, ethylene glycol, the ratio of deionized water are 0.5g：30mL：20mL；
B. by zinc chloride and Fe (NO3)3·9H2O is added to the water, and is adjusted after dissolving using 2mol/L sodium hydroxide solution
It is 8 to save pH value, obtains suspension；Wherein, zinc chloride and Fe (NO3)3·9H2O mol ratio is 1：0.5, Fe (NO3)3·9H2O
Ratio with water is 1.0g：30mL；
C. the carbon quantum dot aqueous solution is added in suspension, 1d is stood after stirring, then hydro-thermal is anti-at 80 DEG C
10h is answered, deionized water and ethanol washing, 50 DEG C of drying is then respectively adopted, obtains carbon quantum dot/zinc ferrite composite photocatalyst material
Material；Wherein, the volume ratio of the carbon quantum dot aqueous solution and suspension is 0.1mL：30mL.
Embodiment 6
A. ascorbic acid is added in ethylene glycol and the mixed solution of deionized water, it is anti-at 200 DEG C after stirring
1h is answered, obtains the carbon quantum dot aqueous solution；Wherein, ascorbic acid, ethylene glycol, the ratio of deionized water are 2g：5mL：10mL；
B. by zinc acetate and Fe (NO3)3·9H2O is added to the water, and is adjusted after dissolving using 2mol/L sodium hydroxide solution
It is 9 to save pH value, obtains suspension；Wherein, zinc acetate and Fe (NO3)3·9H2O mol ratio is 1：5, Fe (NO3)3·9H2O with
The ratio of water is 3.0g：50mL；
C. the carbon quantum dot aqueous solution is added in suspension, 1d is stood after stirring, then hydro-thermal is anti-at 180 DEG C
4h is answered, deionized water and ethanol washing, 60 DEG C of drying is then respectively adopted, obtains carbon quantum dot/zinc ferrite composite photocatalyst material
Material；Wherein, the volume ratio of the carbon quantum dot aqueous solution and suspension is 5mL：50mL.
Embodiment 7
A. ascorbic acid is added in ethylene glycol and the mixed solution of deionized water, it is anti-at 120 DEG C after stirring
3h is answered, obtains the carbon quantum dot aqueous solution；Wherein, ascorbic acid, ethylene glycol, the ratio of deionized water are 5g：20mL：36mL；
B. by zinc nitrate and Fe (NO3)3·9H2O is added to the water, and is adjusted after dissolving using 2mol/L sodium hydroxide solution
It is 11 to save pH value, obtains suspension；Wherein, zinc nitrate and Fe (NO3)3·9H2O mol ratio is 1：1.5, Fe (NO3)3·9H2O
Ratio with water is 2.0g：10mL；
C. the carbon quantum dot aqueous solution is added in suspension, 1d is stood after stirring, then hydro-thermal is anti-at 120 DEG C
8h is answered, deionized water and ethanol washing, 70 DEG C of drying is then respectively adopted, obtains carbon quantum dot/zinc ferrite composite photocatalyst material
Material；Wherein, the volume ratio of the carbon quantum dot aqueous solution and suspension is 25mL：10mL.
Embodiment 8
A. ascorbic acid is added in ethylene glycol and the mixed solution of deionized water, it is anti-at 180 DEG C after stirring
2h is answered, obtains the carbon quantum dot aqueous solution；Wherein, ascorbic acid, ethylene glycol, the ratio of deionized water are 3g：10mL：50mL；
B. by zinc chloride and Fe (NO3)3·9H2O is added to the water, and is adjusted after dissolving using 2mol/L sodium hydroxide solution
It is 14 to save pH value, obtains suspension；Wherein, zinc chloride and Fe (NO3)3·9H2O mol ratio is 1：3.5, Fe (NO3)3·9H2O
Ratio with water is 5.0g：20mL；
C. the carbon quantum dot aqueous solution is added in suspension, 2d is stood after stirring, then hydro-thermal is anti-at 150 DEG C
7h is answered, deionized water and ethanol washing, 100 DEG C of drying is then respectively adopted, obtains carbon quantum dot/zinc ferrite composite photocatalyst material
Material；Wherein, the volume ratio of the carbon quantum dot aqueous solution and suspension is 0.8mL：20mL.
Embodiment 9
A. ascorbic acid is added in ethylene glycol and the mixed solution of deionized water, it is anti-at 110 DEG C after stirring
4h is answered, obtains the carbon quantum dot aqueous solution；Wherein, ascorbic acid, ethylene glycol, the ratio of deionized water are 4g：25mL：40mL；
B. by zinc chloride and Fe (NO3)3·9H2O is added to the water, used after dissolving 2mol/L ammoniacal liquor adjust pH value for
12, obtain suspension；Wherein, zinc chloride and Fe (NO3)3·9H2O mol ratio is 1：0.8, Fe (NO3)3·9H2O and water ratio
For 4.0g：45mL；
C. the carbon quantum dot aqueous solution is added in suspension, 2d is stood after stirring, then hydro-thermal is anti-at 160 DEG C
6h is answered, deionized water and ethanol washing, 90 DEG C of drying is then respectively adopted, obtains carbon quantum dot/zinc ferrite composite photocatalyst material
Material；Wherein, the volume ratio of the carbon quantum dot aqueous solution and suspension is 15mL：45mL.
The invention discloses a kind of simple hydrothermal synthesis of carbon quantum dot/zinc ferrite (CQDs/ZnFe2O4) complex light urges
Agent, carbon quantum dot/zinc ferrite composite photocatalyst material is applied to photocatalytic degradation nitrogen oxides (NOx).Research is found
Under the optimum amount of carbon quantum dot, the structure of carbon quantum dot/zinc ferrite composite photo-catalyst is identical with pure zinc ferrite, is all point
Spinel structure；Zinc ferrite is the ball shaped nano that average particle size is 10nm in carbon quantum dot/zinc ferrite composite photo-catalyst
Grain, carbon quantum dot are distributed in the surface of zinc ferrite；And carbon quantum dot/zinc ferrite composite photo-catalyst is right in visible-range
NOxClearance be up to 38%, it is higher than pure zinc ferrite by 9%, and the intermediate product NO that toxicity is larger2Growing amount it is lower,
Therefore carbon quantum dot/zinc ferrite composite photo-catalyst is to NOxWith higher clearance；When carbon quantum dot/zinc ferrite complex light
When catalyst recycles six times, to NOxPhotocatalytic activity do not change, illustrate that carbon quantum dot/zinc ferrite is multiple
Closing light catalyst is efficient, environmentally friendly photochemical catalyst, and preparation method is simple, and raw material is cheap to be easy to get, and has wide answer
Use prospect.
It should be noted that the invention is not limited in any way for above-described embodiment, it is all to use equivalent substitution or equivalent change
The technical scheme that the mode changed is obtained, all falls within protection scope of the present invention.
Claims (7)
1. the preparation method of a kind of carbon quantum dot/zinc ferrite composite photocatalyst material, it is characterised in that comprise the following steps：
A. ascorbic acid is added in ethylene glycol and the mixed solution of deionized water, it is anti-at 100-200 DEG C after stirring
1-5h is answered, obtains the carbon quantum dot aqueous solution；Wherein, ascorbic acid, ethylene glycol, the ratio of deionized water are (0.5-5.0) g：(5.0-
30)mL：(10-50)mL；
B. by zinc salt and Fe (NO3)3·9H2O is added to the water, and it is 8-14 that pH value is adjusted after dissolving, obtains suspension；Wherein, zinc
Salt and Fe (NO3)3·9H2O mol ratio is 1：(0.1-5.0), Fe (NO3)3·9H2The ratio of O and water is (1.0-5.0) g：(10-
50)mL；
C. the carbon quantum dot aqueous solution is added in suspension, stood after stirring, then the hydro-thermal reaction at 80-180 DEG C
4-10h, it is washed out, dries, obtains carbon quantum dot/zinc ferrite composite photocatalyst material；Wherein, the carbon quantum dot aqueous solution is with hanging
The volume ratio of supernatant liquid is (0.1-25) mL：(10-50)mL.
2. a kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 1, its feature exist
In zinc salt is zinc nitrate, zinc chloride or zinc acetate in the step b.
3. a kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 1, its feature exist
In using sodium hydroxide solution or ammonia spirit regulation pH value in the step b.
4. a kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 3, its feature exist
In the sodium hydroxide solution, the concentration of ammonia spirit are 2mol/L.
5. a kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 1, its feature exist
In the time stood in the step c is 1 day.
6. a kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 1, its feature exist
In, in the step c washing be specially：Deionized water and ethanol washing is respectively adopted.
7. a kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 1, its feature exist
In the temperature dried in the step c is 50-100 DEG C.
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