CN108404926A - A kind of unbodied ferric vandate/pucherite/graphene composite photocatalyst and its preparation method and application - Google Patents
A kind of unbodied ferric vandate/pucherite/graphene composite photocatalyst and its preparation method and application Download PDFInfo
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- CN108404926A CN108404926A CN201810146379.5A CN201810146379A CN108404926A CN 108404926 A CN108404926 A CN 108404926A CN 201810146379 A CN201810146379 A CN 201810146379A CN 108404926 A CN108404926 A CN 108404926A
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- 239000002131 composite material Substances 0.000 title claims abstract description 69
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 62
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 47
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 36
- 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 22
- 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 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- 235000011187 glycerol Nutrition 0.000 claims abstract description 18
- 230000001699 photocatalysis Effects 0.000 claims abstract description 17
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 11
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 11
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 11
- 239000002351 wastewater Substances 0.000 claims abstract description 11
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 238000010531 catalytic reduction reaction Methods 0.000 claims abstract description 5
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 238000002604 ultrasonography Methods 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- DJQWBIAOLCVTJU-UHFFFAOYSA-O [Bi].[N+](=O)([O-])[O-].[NH4+] Chemical compound [Bi].[N+](=O)([O-])[O-].[NH4+] DJQWBIAOLCVTJU-UHFFFAOYSA-O 0.000 claims description 2
- 238000005352 clarification Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- LITYQKYYGUGQLY-UHFFFAOYSA-N iron nitric acid Chemical compound [Fe].O[N+]([O-])=O LITYQKYYGUGQLY-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 6
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000011651 chromium Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 9
- 238000007146 photocatalysis Methods 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000000908 ammonium hydroxide Substances 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000008236 heating water Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 229910002915 BiVO4 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000021615 conjugation Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910052742 iron Inorganic materials 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
- 230000031700 light absorption Effects 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- XDBSEZHMWGHVIL-UHFFFAOYSA-M hydroxy(dioxo)vanadium Chemical compound O[V](=O)=O XDBSEZHMWGHVIL-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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- 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
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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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8472—Vanadium
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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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- B01J35/61—Surface area
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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- C02F2101/00—Nature of the contaminant
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Abstract
The invention belongs to nanocomposite technical field, a kind of unbodied ferric vandate/pucherite/graphene composite photocatalyst and its preparation method and application is specifically disclosed.Steps are as follows for the preparation method：The glycerin solution of bismuth nitrate, graphene powder, ammonium metavanadate aqueous solution and iron nitrate solution are mixed to get precursor solution; carry out hydro-thermal reaction; ascorbic acid solution is added and stands under inert gas protection; it is alternately washed with absolute ethyl alcohol and deionized water, obtains unbodied ferric vandate/pucherite/graphene composite photocatalyst after drying.50nm is less than using amorphous ferric vandate/pucherite/graphene composite photocatalyst grain size that the above method is prepared, with larger specific surface area, its photocatalytic activity is also considerably beyond pure pucherite or ferric vandate, it can be used in photo catalytic reduction Cr (VI) and the advanced treating of chromate waste water, have broad application prospects.
Description
Technical field
The present invention relates to nanocomposite technical fields, and in particular, to and a kind of unbodied ferric vandate/pucherite/
Graphene composite photocatalyst and its preparation method and application.
Background technology
With the fast development of global economy, problem of environmental pollution becomes increasingly conspicuous, and heavy metal pollution is particularly acute.Wherein,
Containing chromium（Typically Cr (VI)）Organic wastewater pollution is mainly derived from commercial pigments waste water, leather preparation waste water, electroplating wastewater etc.,
Such biochemical degree of waste water is low, and intractability is big, and the catalyst used in high-level oxidation technology at present, often can only be single
Ground handles organic pollution, the ability without having both the heavy metals such as processing Cr VI.In traditional technology research, it is with titanium dioxide
The Photocatalitic Technique of Semiconductor that core represents is widely used in field of environment pollution control, but the band gap width of titanium dioxide is
3.2eV only has reaction, practicability poor under ultraviolet light.Therefore, existing to administer the pollution problem of the organic wastewater containing chromium
Urgently develop a kind of novel photocatalyst for Cr (VI) that can effectively degrade under visible light.
Pucherite is primarily present three kinds of crystal forms as a kind of semiconductor having visible light response activity：Cubic Zircon cut
（zt）, cubic scheelite type（s-t）, monocline scheelite type（s-m）.Wherein, the energy gap of monoclinic phase pucherite is about
2.40eV, it is seen that light induced electron and photohole can be generated under illumination, there is excellent chemical stability, nothing in aqueous solution
It poisons and manufacturing cost is low.Pucherite has wide hair in technical fields such as degradable organic pollutant, photolysis water hydrogen oxygen
Exhibition foreground.But pure phase pucherite itself there are still photo-generated carrier easily compound, adsorption energy force difference the shortcomings that.
Carbon atom in graphene is arranged in hexa-atomic loop type in monoatomic layer plane, and there are four the C of valence electron originals for tool
The valence electron of son one non-bonding of contribution.These valence electrons direction vertical with plane in the two dimensional crystal structure of monoatomic layer
The big key of delocalization of conjugation is formed, therefore electronics can move freely in crystal, enables graphene that there is excellent electronic conductivity.
In addition, graphene also has excellent mechanical performance and high-permeability and high-specific surface area to light, can be used to prepare graphite
Alkene various functions composite material.Graphene performance outstanding and its workability make it in photocatalysis field have well to answer
With foreground, light induced electron can be quickly transmitted to material surface, efficiently separate light induced electron-by excellent electric conductivity
Hole pair reduces their recombination rate.
Existing research it has proven convenient that can promote pucherite crystal to a certain extent in a small amount of graphene of pucherite area load
{ 010 } preferred growth of the preferred growth of crystal face, the crystal face helps to improve the separative efficiency of photo-generate electron-hole pair.Meanwhile
Graphene surface, which exists, is largely originated from sp2The conjugation carbon network of connection removes localized electronic, thus has good electric conductivity, energy
Further speed up conduction of the photo-generated carrier in pucherite composite material surface.But pucherite-the graphene reported at present
Composite material is mostly the crystalline structure of rule, and for particle size also mostly between 100~200nm, specific surface area is smaller, photocatalysis
Performance is still to be improved；And as amorphous amorphous composite material, then generally existing crystallite dimension is larger, adsorption energy force difference,
Photo-generated carrier is difficult to detach, and electron hole pair is easy compound so that the lower defect of photocatalysis efficiency.
Invention content
The purpose of the invention is to overcome the above-mentioned deficiency of the prior art, a kind of unbodied ferric vandate/vanadic acid is provided
The preparation method of bismuth/graphene composite photocatalyst is less than 50nm by the composite photo-catalyst grain size that this method is prepared,
With higher specific surface area, photocatalytic activity is also considerably beyond pure pucherite or ferric vandate.
Another object of the present invention is to provide a kind of unbodied ferric vandate/pucherite/graphene composite photocatalysts.
Another object of the present invention is to provide above-mentioned unbodied ferric vandate/pucherite/graphene composite photocatalysts
Application in photo catalytic reduction Cr (VI) and/or the advanced treating of chromate waste water.
To achieve the goals above, the present invention is achieved by following scheme：
A kind of preparation method of unbodied ferric vandate/pucherite/graphene composite photocatalyst, includes the following steps：
S1. graphene powder, ultrasound, 10~15min of stirring is added in the glycerin solution for preparing bismuth nitrate；
S2. ammonium metavanadate aqueous solution and iron nitrate solution are prepared；By the glycerin solution and nitric acid of treated in S1 bismuth nitrate
Ammonium metavanadate aqueous solution is added in ferrous solution mixing after clarification, stir 15~30min, adjusts pH value to 4~7, it is molten to obtain presoma
Liquid is stood, 1~2h of aging；
S3. constant temperature carries out 10~20h of hydro-thermal reaction under the conditions of precursor solution obtained by S2 being placed in 158~162 DEG C, obtains bright orange
Color suspension；
S4. glassy yellow suspension obtained by S3 is stood into 10~30min, after discarding 1/2 volume supernatant, it is molten that ascorbic acid is added
Liquid stands 0.5~1h under inert gas protection；With alternately washing 3 times of absolute ethyl alcohol and deionized water, in 60 DEG C dry 10~
20h is to get to unbodied ferric vandate/pucherite/graphene composite photocatalyst.
Since amorphous amorphous composite material has that photo-generated carrier is difficult to detach, and improve photoproduction current-carrying
The method of sub- separative efficiency includes noble metal loading, forms hetero-junctions etc. with other semiconductors couplings.It is prepared by present invention selection
The ferric vandate of suitable proportion is added in the process, and the band gap of ferric vandate is 2.05eV, ferric vandate valence band and conduction band positions and vanadic acid
Bismuth matches, and can form hetero-junctions between the two.
More specific principle is as follows：Comprising by Bi 6s and O the 2p hybridized orbits formed and V 3d rails in pucherite energy band
The conduction band of road composition, thus band gap reduces, and visible region is extended to the absorption of light.Vanadic acid iron rule has narrower energy band
Gap, the spectral band absorbed extend to the visible region of bigger.Precursor solution containing pucherite and ferric vandate is having third
The amorphous samples that hydro-thermal reaction generation is carried out in the environment of triol, compared with pure pucherite or ferric vandate, first, because without fixed
The interfacial effect of the pucherite of shape/ferric vandate hetero-junctions（Built in field accelerates photo-generate electron-hole to dividing mainly between interface
From）It being formed, band gap is down to 1.85eV at the two contact interface, and light absorption area further expands near infrared region, to 500~
Light within the scope of 800nm has stronger absorption, photo-generate electron-hole to be improved to largely migrating to photocatalysis composite surface
Light induced electron and photohole and pollutant contact probability, to improve the photocatalytic activity of composite material；Second is that amorphous
Aspect product nanoparticle size an order of magnitude smaller than crystalline state sample or so, thus its specific surface area compares the vanadic acid of crystalline state
Bismuth or ferric vandate bigger have more active sites, can more contact the pollutant in water body.Wherein, composite photocatalyst
The Cr of agent material adsorption2O7 2-As light induced electron receptor, it is reduced to the Cr (III) of low toxicity, further promotes photoproduction
The separation of electron hole pair promotes photohole more to touch the small organic molecule for being adsorbed in material surface, by its oxygen
Change degradation.
Therefore, the present invention is molten by the glycerine of iron nitrate solution, bismuth nitrate using graphene as conductive film and growth templates
Liquid is mixed with ammonium metavanadate aqueous solution according to certain molar ratio, is reacted by conventional hydrothermal, and grain size is prepared and is less than 50nm
Amorphous ferric vandate/pucherite/graphene composite photocatalyst, pucherite/ferric vandate heterojunction structure had both been utilized（p-n
Hetero-junctions）Promote the separation and conduction of photo-generated carrier with graphene conductive layer so that excitation generates under visible light illumination
The separation rate of photo-generate electron-hole pair greatly improve；Also amorphous, the distinctive large specific surface area of impalpable structure are utilized, from
And increase composite photo-catalyst itself and Cr in water body (VI) contact surface, so that composite photo-catalyst is possessed than general crystalline material
More photocatalytic activity sites, greatly improve the photocatalysis performance of composite photocatalyst material.
Preferably, in the glycerin solution of the bismuth nitrate, a concentration of 30~60mmol/L of bismuth nitrate；The metavanadic acid
A concentration of 60~100mmol/L of aqueous ammonium；A concentration of 30~60mmol/L of the iron nitrate solution；The ascorbic acid
A concentration of 0.2mol/L of solution.
It is highly preferred that in the glycerin solution of the bismuth nitrate, a concentration of 40mmol/L of bismuth nitrate；The ammonium metavanadate
A concentration of 80mmol/L of aqueous solution；A concentration of 40mmol/L of the iron nitrate solution.
Preferably, the glycerin solution of the bismuth nitrate, ammonium metavanadate aqueous solution, iron nitrate solution, ascorbic acid solution
Volume ratio be followed successively by 5~20：10~20：4~8：2~5.It is highly preferred that the glycerin solution of the bismuth nitrate, ammonium metavanadate
Aqueous solution, iron nitrate solution, ascorbic acid solution volume be respectively 50~200mL, 100~200mL, 40~80mL, 20~
50mL。
Preferably, the mass ratio of bismuth nitrate described in S1 and graphene powder is 1.94：0.004~0.032.
Preferably, the temperature that ammonium metavanadate aqueous solution is prepared described in S2 is 60~90 DEG C.It is highly preferred that matching described in S2
The temperature of ammonium metavanadate aqueous solution processed is 70~80 DEG C.
Preferably, adjusted described in S2 pH value the specific steps are adjust pH value to 6 with ammonium hydroxide.
Preferably, hydro-thermal reaction described in S3 carries out in the stainless steel autoclave with Teflon liners.
Preferably, the hydro-thermal reaction time described in S3 is 12h.
The bismuth nitrate is Bi (NO3)3•5H2O, ferric nitrate are Fe (NO3)3•9H2O, pucherite BiVO4, ferric vandate
For FeVO4。
A kind of unbodied ferric vandate/pucherite/graphene composite photocatalyst is also claimed in the present invention, by above-mentioned side
Method is prepared, and grain size is less than 50nm；Wherein, the molar ratio of pucherite and ferric vandate is 1~4：1, the quality hundred of graphene
Score is 0.5~2.4%.
There is a stronger absorption in composite photo-catalyst Uv and visible light area, pucherite and vanadium in composite photo-catalyst
The molar ratio of sour iron is 1：1、2：1、3：1、4：1 band gap is respectively 2.23eV, 1.98eV, 2.09eV, 2.06eV, respectively less than
The band gap of pucherite（2.40eV）；Wherein, pucherite and ferric vandate molar ratio are 2：1 composite photo-catalyst band-gap energy is most
It is small, it is less than the band gap of pure ferric vandate（2.05eV）, therefore the composite photo-catalyst being prepared is rung with good visible light
Answer performance.
Unbodied ferric vandate/pucherite/graphene composite photocatalyst provided by the present invention contains sexavalence in photocatalysis
In the experiment of the combined pollutant of chromium, pucherite：Ferric vandate molar ratio is 1：The photo catalytic reduction sexavalence of 1 composite sample
Chromium effect is best, reaches 90% to the removal rate of Cr (VI) in 180min.
Therefore, above-mentioned unbodied ferric vandate/pucherite/graphene composite photocatalyst is also claimed in light in the present invention
Catalysis restores the application in Cr (VI) and/or the advanced treating of chromate waste water.
Compared with prior art, the invention has the advantages that：
Amorphous ferric vandate/pucherite/graphene composite photocatalyst of the present invention, it is heterogeneous to be both utilized pucherite/ferric vandate
Junction structure（P-n heterojunction）Promote the separation and conduction of photo-generated carrier with graphene conductive layer so that in radiation of visible light
The separation rate for the photo-generate electron-hole pair that lower excitation generates greatly improves；Also amorphous, the distinctive larger ratio of impalpable structure are utilized
Surface area makes composite photo-catalyst than general knot to increase composite photo-catalyst itself and Cr in water body (VI) contact surface
Brilliant material possesses more photocatalytic activity sites, greatly improves the photocatalysis performance of composite photocatalyst material, can be used for
In photo catalytic reduction Cr (VI) and the advanced treating of chromate waste water, have broad application prospects.
Description of the drawings
Fig. 1 is the finished figure of ferric vandate/pucherite/graphene composite photocatalyst prepared by the present invention.
Fig. 2 is the XRD diffraction patterns of ferric vandate/pucherite/graphene composite photocatalyst prepared by the present invention；Wherein, a is
1 gained composite photo-catalyst of embodiment, b are 2 gained composite photo-catalyst of embodiment, and c is 3 gained composite photocatalyst of embodiment
Agent.
Fig. 3 is the TEM electron microscopes of ferric vandate/pucherite/graphene composite photocatalyst prepared by the present invention.
Fig. 4 is the UV-vis absorption spectrums of ferric vandate/pucherite/graphene composite photocatalyst prepared by the present invention；Its
In, a is 1 gained composite photo-catalyst of embodiment, and b is 2 gained composite photo-catalyst of embodiment, and c is 3 gained complex light of embodiment
Catalyst.
Fig. 5 is the ferric vandate/pucherite/graphene composite photocatalyst of the invention prepared under visible light to Cr's (VI)
Also virgin curve；Wherein, a is 1 gained composite photo-catalyst of embodiment, and b is 2 gained composite photo-catalyst of embodiment, and c is embodiment
3 gained composite photo-catalysts.
Specific implementation mode
With reference to the accompanying drawings of the specification and specific embodiment is made the present invention and is further elaborated, the embodiment
It is served only for explaining the present invention, be not intended to limit the scope of the present invention.Test method used in following embodiments is such as without spy
Different explanation, is conventional method；Used material, reagent etc., unless otherwise specified, for the reagent commercially obtained
And material.
Embodiment 1
A kind of preparation method of unbodied ferric vandate/pucherite/graphene composite photocatalyst, includes the following steps：
1,1.94g Bi (NO accurately are weighed3)3•5H2O is added in 80mL glycerine, and 0.032g stones are added in ultrasound, dispersion 10min
Black alkene powder continues ultrasound, stirring 10min；
2,0.94g NH accurately are weighed4VO3, it is added in 100mL deionized waters, heating water bath, stirring are until white at 80 DEG C
Powder is completely dissolved；
3,1.62g Fe (NO accurately are weighed3)3•9H2O is dissolved in 50mL deionized waters, is added into step 1 gained bismuth nitrate
In glycerin solution, after stirring makes it uniformly clarify, under magnetic stirring, step 2 gained ammonium metavanadate aqueous solution is added dropwise,
Stirring 20min is then proceeded to, pH value is adjusted to 6 with ammonium hydroxide, obtains precursor solution, stand at room temperature, aging 1h；
4, step 3 gained precursor solution is transferred in the stainless steel autoclave with Telflon liners, it is permanent at 160 DEG C
Temperature carries out hydro-thermal reaction 12h, obtains glassy yellow suspension；
5, step 4 gained glassy yellow suspension is stood into 20min, after discarding 1/2 volume supernatant, 40mL 0.2mol/L is added
Ascorbic acid solution stands 1h under the protection of inert gas；It is alternately washed 3 times with absolute ethyl alcohol and deionized water, in 60 DEG C
Dry 10h is to get to unbodied ferric vandate/pucherite/graphene composite photocatalyst powder in baking oven.It is obtained compound
The mass percent of graphene is 1.6wt% in photochemical catalyst（Theoretical calculation）, ferric vandate：Pucherite molar ratio is 1:1.
Embodiment 2
A kind of preparation method of unbodied ferric vandate/pucherite/graphene composite photocatalyst, includes the following steps：
1,1.94g Bi (NO accurately are weighed3)3•5H2O is added in 80mL glycerine, and 0.016g stones are added in ultrasound, dispersion 10min
Black alkene powder continues ultrasound, stirring 10min；
2,0.94g NH accurately are weighed4VO3, it is added in 100mL deionized waters, heating water bath, stirring are until white at 80 DEG C
Powder is completely dissolved；
3,1.62g Fe (NO accurately are weighed3)3•9H2O is dissolved in 50mL deionized waters, is added into step 1 gained bismuth nitrate
In glycerin solution, after stirring makes it uniformly clarify, under magnetic stirring, step 2 gained ammonium metavanadate aqueous solution is added dropwise,
Stirring 20min is then proceeded to, pH value is adjusted to 6 with ammonium hydroxide, obtains precursor solution, stand at room temperature, aging 1h；
4, step 3 gained precursor solution is transferred in the stainless steel autoclave with Telflon liners, it is permanent at 160 DEG C
Temperature carries out hydro-thermal reaction 12h, obtains glassy yellow suspension；
5, step 4 gained glassy yellow suspension is stood into 20min, after discarding 1/2 volume supernatant, 40mL 0.2mol/L is added
Ascorbic acid solution stands 1h under the protection of inert gas；It is alternately washed 3 times with absolute ethyl alcohol and deionized water, in 60 DEG C
Dry 10h is to get to unbodied ferric vandate/pucherite/graphene composite photocatalyst powder in baking oven.It is obtained compound
The mass percent of graphene is 0.8wt% in photochemical catalyst（Theoretical calculation）, ferric vandate：Pucherite molar ratio is 1:1.
Embodiment 3
A kind of preparation method of unbodied ferric vandate/pucherite/graphene composite photocatalyst, includes the following steps：
1,1.94g Bi (NO accurately are weighed3)3•5H2O is added in 80mL glycerine, and 0.032g stones are added in ultrasound, dispersion 10min
Black alkene powder continues ultrasound, stirring 10min；
2,1.4g NH accurately are weighed4VO3, it is added in 100mL deionized waters, heating water bath, stirring are until white powder at 80 DEG C
End is completely dissolved；
3,1.62g Fe (NO accurately are weighed3)3•9H2O is dissolved in 50mL deionized waters, is added into step 1 gained bismuth nitrate
In glycerin solution, after stirring makes it uniformly clarify, under magnetic stirring, step 2 gained ammonium metavanadate aqueous solution is added dropwise,
Stirring 20min is then proceeded to, pH value is adjusted to 6 with ammonium hydroxide, obtains precursor solution, stand at room temperature, aging 1h；
4, step 3 gained precursor solution is transferred in the stainless steel autoclave with Telflon liners, it is permanent at 160 DEG C
Temperature carries out hydro-thermal reaction 12h, obtains glassy yellow suspension；
5, step 4 gained glassy yellow suspension is stood into 20min, after discarding 1/2 volume supernatant, 40mL 0.2mol/L is added
Ascorbic acid solution stands 1h under the protection of inert gas；It is alternately washed 3 times with absolute ethyl alcohol and deionized water, in 60 DEG C
Dry 10h is to get to unbodied ferric vandate/pucherite/graphene composite photocatalyst powder in baking oven.It is obtained compound
The mass percent of graphene is 0.96wt% in photochemical catalyst（Theoretical calculation）, ferric vandate：Pucherite molar ratio is 1:2.
The appearance of final products is as shown in Figure 1, the presentation of prepared composite photo-catalyst is dark green obtained by Examples 1 to 3
Color, quality is fluffy easily to be ground.
The X-ray diffractogram of composite photo-catalyst obtained by Examples 1 to 3（XRD）As shown in Fig. 2, be shown in 2 Theta=
There are one " steamed bun peaks " at 25~30 °, do not show any FeVO4And BiVO4Related characteristic peak, show sample in amorphous,
Amorphous state.
The transmission electron microscope picture of the composite photo-catalyst（TEM）As shown in figure 3, can be clearly seen from figure, grain size<
The tiny spherical nanoparticle of 50nm is wrapped up by graphene, and in light-catalyzed reaction, graphene can admirably conduct photoproduction electricity
Son.
The solid UV-Vis DRS of the composite photo-catalyst（UV-vis）Absorption spectrum is as shown in figure 4, accordingly
Estimation, the band gap corresponding to the composite photo-catalyst described in Examples 1 to 3 is respectively 2.27eV, 2.14eV, 2.12eV, table
Bright prepared composite photo-catalyst has good visible light-responded performance.
Application examples
Amorphous ferric vandate/pucherite/graphene composite photocatalyst obtained by 0.1g Examples 1 to 3 is taken respectively, is added to
250mL K containing 5mg/L2Cr2O7In the mixed solution for the methanol for being 0.2% with volume content, magnetic agitation is carried out, with low wattage
（30W）White light LEDs are visible light source, when progress a length of 180min light-catalyzed reaction.
Composite photo-catalyst obtained by Examples 1 to 3 is as shown in Figure 5 to the reduction effect of Cr (VI)：Where it can be seen that
Composite photo-catalyst prepared by embodiment 1 reaches 90% or more in 180min to Cr (VI) removal rate, the higher amount having
Sub- efficiency.Sacrifice agent of the methanol of low concentration as photohole in solution, it is suppressed that the light induced electron and light of catalyst surface
Raw hole-recombination promotes the separation of photo-generate electron-hole pair, highly toxic Cr under the hetero-junctions collective effect of material internal
(VI) it is adsorbed to composite photo-catalyst surface, the Cr (III) of low toxicity is reduced to as light induced electron receptor.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is protected to the present invention
The limitation of shield range can also be made on the basis of above description and thinking for those of ordinary skill in the art
Other various forms of variations or variation, there is no necessity and possibility to exhaust all the enbodiments.It is all the present invention
All any modification, equivalent and improvement etc., should be included in the protection of the claims in the present invention made by within spirit and principle
Within the scope of.
Claims (10)
1. a kind of preparation method of unbodied ferric vandate/pucherite/graphene composite photocatalyst, which is characterized in that including
Following steps：
S1. graphene powder, ultrasound, 10~15min of stirring is added in the glycerin solution for preparing bismuth nitrate；
S2. ammonium metavanadate aqueous solution and iron nitrate solution are prepared；By the glycerin solution and nitric acid of treated in S1 bismuth nitrate
Ammonium metavanadate aqueous solution is added in ferrous solution mixing after clarification, stir 15~30min, adjusts pH value to 4~7, it is molten to obtain presoma
Liquid is stood, 1~2h of aging；
S3. constant temperature carries out 10~20h of hydro-thermal reaction under the conditions of precursor solution obtained by S2 being placed in 158~162 DEG C, obtains bright orange
Color suspension；
S4. glassy yellow suspension obtained by S3 is stood into 10~30min, after discarding 1/2 volume supernatant, it is molten that ascorbic acid is added
Liquid stands 0.5~1h under inert gas protection；With alternately washing 3 times of absolute ethyl alcohol and deionized water, in 60 DEG C dry 10~
20h is to get to unbodied ferric vandate/pucherite/graphene composite photocatalyst.
2. preparation method according to claim 1, which is characterized in that in the glycerin solution of the bismuth nitrate, bismuth nitrate
A concentration of 30~60mmol/L；A concentration of 60~100mmol/L of the ammonium metavanadate aqueous solution；The iron nitrate solution
A concentration of 30~60mmol/L；A concentration of 0.2mol/L of the ascorbic acid solution.
3. preparation method according to claim 2, which is characterized in that glycerin solution, the ammonium metavanadate of the bismuth nitrate
Aqueous solution, iron nitrate solution, ascorbic acid solution volume ratio be followed successively by 5~20：10~20：4~8：2~5.
4. preparation method according to claim 1, which is characterized in that the quality of bismuth nitrate described in S1 and graphene powder
Than being 1.94：0.004~0.032.
5. preparation method according to claim 1, which is characterized in that prepare the temperature of ammonium metavanadate aqueous solution described in S2
It is 60~90 DEG C.
6. preparation method according to claim 5, which is characterized in that prepare the temperature of ammonium metavanadate aqueous solution described in S2
It is 70~80 DEG C.
7. preparation method according to claim 1, which is characterized in that adjusted described in S2 pH value the specific steps are with ammonia
Water adjusts pH value to 6.
8. preparation method according to claim 1, which is characterized in that the bismuth nitrate is Bi (NO3)3•5H2O, nitric acid
Iron is Fe (NO3)3•9H2O。
9. a kind of unbodied ferric vandate/pucherite/graphene composite photocatalyst, which is characterized in that by claim 1 to 8
Any one preparation method is prepared, and grain size is less than 50nm；Wherein, the molar ratio of pucherite and ferric vandate is 1~4：
1, the mass percent of graphene is 0.5~2.4%.
10. unbodied ferric vandate/pucherite/graphene composite photocatalyst is in photo catalytic reduction Cr described in claim 9
(VI) application and/or in the advanced treating of chromate waste water.
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| CN111081999A (en) * | 2019-11-27 | 2020-04-28 | 武汉理工大学 | Potassium vanadate/reduced graphene electrode material and preparation method and application thereof |
| CN114904534A (en) * | 2022-05-19 | 2022-08-16 | 福州大学 | Bismuth molybdate/ferric vanadate composite nanomaterial, preparation method thereof and application thereof in acousto-optic catalytic degradation of pollutants in water |
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