CN107185547A - A kind of C/Fe FeVO4Composite photo-catalyst and its preparation method and application - Google Patents
A kind of C/Fe FeVO4Composite photo-catalyst and its preparation method and application Download PDFInfo
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- CN107185547A CN107185547A CN201710420771.XA CN201710420771A CN107185547A CN 107185547 A CN107185547 A CN 107185547A CN 201710420771 A CN201710420771 A CN 201710420771A CN 107185547 A CN107185547 A CN 107185547A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002131 composite material Substances 0.000 claims abstract description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910001868 water Inorganic materials 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 229960003405 ciprofloxacin Drugs 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 14
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 11
- 239000008103 glucose Substances 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 claims abstract description 11
- 229910003206 NH4VO3 Inorganic materials 0.000 claims abstract description 10
- 235000019441 ethanol Nutrition 0.000 claims abstract description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 10
- 239000010935 stainless steel Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 235000013924 ferrous gluconate Nutrition 0.000 claims abstract description 9
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 8
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims abstract description 7
- 229960001645 ferrous gluconate Drugs 0.000 claims abstract description 6
- 239000004222 ferrous gluconate Substances 0.000 claims abstract description 6
- VRIVJOXICYMTAG-IYEMJOQQSA-L iron(ii) gluconate Chemical compound [Fe+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O VRIVJOXICYMTAG-IYEMJOQQSA-L 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000013049 sediment Substances 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- 229960001180 norfloxacin Drugs 0.000 claims abstract description 5
- OGJPXUAPXNRGGI-UHFFFAOYSA-N norfloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNCC1 OGJPXUAPXNRGGI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 238000002604 ultrasonography Methods 0.000 claims description 7
- -1 afterwards Substances 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000527 sonication Methods 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000001291 vacuum drying Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 37
- 239000003054 catalyst Substances 0.000 description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 230000000694 effects Effects 0.000 description 9
- 230000003197 catalytic effect Effects 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 238000005755 formation reaction Methods 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 150000002823 nitrates Chemical class 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 235000003283 Pachira macrocarpa Nutrition 0.000 description 2
- 241001083492 Trapa Species 0.000 description 2
- 235000014364 Trapa natans Nutrition 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 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
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 235000009165 saligot Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 229940124307 fluoroquinolone Drugs 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
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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
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/038—Precipitation; Co-precipitation to form slurries or suspensions, e.g. a washcoat
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
A kind of C/Fe FeVO4Composite photo-catalyst and its preparation method and application, belongs to technical field of inorganic nano-material preparation.Glucose, ferrous gluconate are mixed, deionized water is added and stirs to clarify and dissolve material, be placed in hydrothermal reaction kettle and react, take out reactor after cooling, washed with deionized water and absolute ethyl alcohol, the sediment vacuum drying after washing is obtained into carbon paste ball；Will be ultrasonically treated in carbon paste ball addition deionized water, take Fe (NO3)3·9H2O、NH4VO3With SDBS surfactants, add after being mixed in carbon paste ball, continue ultrasonically treated, adjust the pH value of solution, obtain grey solution；Grey solution is positioned in stainless steel cauldron, reacted under hydrothermal conditions, room temperature is cooled to, turbid solution is obtained；Turbid solution is centrifuged, washing drying is carried out respectively with water and ethanol, obtains C/Fe FeVO4Presoma；By C/Fe FeVO4Presoma is calcined, and obtains the C/Fe FeVO of meso-porous nano laminated structure composition4.The present invention is used for processing Ciprofloxacin, the application of the emerging micropollutants of Norfloxacin under visible light.
Description
Technical field
The present invention relates to a kind of C/Fe-FeVO4Composite photo-catalyst and its preparation method and application, belongs to inorganic nano material
Expect preparing technical field.
Background technology
Ferric vandate belongs to a kind of n-type semiconductor, FeVO4The novel semi-conductor photochemical catalyst of to be one have direct band gap, can
Carry out degradable organic pollutant to absorb visible ray.Ferric vandate mainly has four kinds of crystal formations：Three oblique types, orthogonal typeOrthogonal typeWith
Monocline type.Wherein three oblique types are made at ambient pressure, and other three kinds of crystal formations must can just be obtained under high pressure conditions.FeVO4Should
For the lithium battery of high-energy-density, photochemical catalyst, in terms of hydrogen catalytic combustion.
FeVO4Semiconductor light-catalyst belongs to visible light-responded photochemical catalyst, researcher to it under visible light
Good photocatalysis performance in depth probed into.However, for FeVO4The research of doping vario-property technology can enter
Modification in its performance of row and crystal formation, can so greatly improve its response range come organic poison of degrading, for FeVO4Mix
The research of miscellaneous modification technology, it is little by little of interest by people.
The synthesizing mean of vanadic acid iron catalyst has solid reaction process, liquid-phase precipitation method, hydrothermal synthesis method and molten at this stage
Glue-gel method etc., using ammonium metavanadate and ferric nitrate as main precursor reactant raw material, photochemical catalyst is prepared with hydrothermal synthesis method
Ferric vandate, and the influence of temperature and the pH value size of solution to crystalline solid ferric vandate when discussing reaction, make synthetic crystallization
Type ferric vandate (FeVO4) sample has theoretical property reference.
The sample shape of solid reaction process formation is thick and uneven, tends to have uncorrelated impurities phase generation, hydrothermal synthesis method
The sample of preparation belongs to orthogonal typeReaction condition requires relatively high, it is necessary to high-temperature and high-pressure conditions, the time of reaction
It is long.Liquid-phase precipitation method generates presoma, produces the oblique type of novel photocatalyst three in different ground temperature lower calcination presoma respectively
FeVO4Photochemical catalyst.This method is not required under high-temperature and high-pressure conditions and prolonged calcining, and precipitation compare it is more uniform, if
Can get hold of in the case of reaction condition can free from admixture mutually produce.The sample prepared to experiment can using XRD, SEM, IR and
The means such as DRS characterize its crystal formation, configuration of surface and light energy absorption performance, and by antibioticses solution of degrading so as to evaluate its light
Catalytic activity.
Under conditions of acid and alkalescence differs, ferric vandate is synthesized as heterogeneous catalysis by the use of hydrothermal synthesis method, is replaced
For conventional homogeneous Fenton system degradating organic dyes, the different condition of synthesis is found to its form, configuration, composition and catalytic
The Different Effects of energy, and study the pH, catalyst concn, H of heterogeneous system2O2The best reaction condition such as concentration, selects sedimentation
Fast and separation is rapid, pH selections field is big, type Fenton catalyst with application value.
Synthesize and use FeVO at present4Photochemical catalyst and apply degraded toxic organic pollutant report still relatively
It is few, but photocatalysis research all has the consumption and H of catalyst2O2Using ultraviolet light, to visible during the universal bigger than normal, photocatalysis of amount
These not high not enough places of light efficiency.In addition, in view of the metallic element that v element enriches as China's storage capacity, is developed
FeVO4Photochemical catalyst is with certain practical significance and bright application prospect.
Publication No. CN103599804A patent document discloses a kind of N-FeVO4/Fe2O3Composite photo-catalyst and its
Preparation method and application, a kind of N-FeVO4/Fe2O3Composite photo-catalyst and its preparation method and application, by ferric chloride (FeCl36H2O)
It is soluble in water to obtain solution A, ammonium metavanadate is dissolved in hot water and obtains solution B, is 1 by Fe and V mol ratio:1 solution B is added to it is molten
Suspension C is obtained in liquid A；Add NaN thereto again3、N2H4·H2O and NH4Cl obtains mixed solution, then carries out hydro-thermal reaction, then
Dry precursor powder, finally calcines to obtain N-FeVO4/Fe2O3Composite photo-catalyst.α of the catalyst including water chestnut square structure-
Fe2O3With the FeVO of three monoclinic phases4, and FeVO4Lattice in contain N element；Its pattern is strip fusiformis structure and/or bulk
Structure, with good photocatalytic activity, can apply to degradation of organic substances under ultraviolet light.The present invention has that technique is simple, behaviour
Make convenience, short preparation period, the advantage that reaction condition is gentle, production efficiency is high.
Publication No. CN103586042A patent document discloses a kind of α-Fe2O3/FeVO4Composite photo-catalyst and its
Preparation method and application, the invention discloses a kind of α-Fe2O3/FeVO4Composite photo-catalyst and its preparation method and application, will
FeCl3·6H2O is soluble in water to obtain solution A, by NH4VO3It is dissolved in hot water and obtains solution B, is 1 according to Fe and V mol ratio:1 will
Solution B, which is added in solution A, obtains mixed liquor, and the pH value of regulation mixed liquor is 5~8, and mixed liquor then is poured into hydrothermal reaction kettle
Middle carry out hydro-thermal reaction, prepares α-Fe2O3/FeVO4Composite photo-catalyst, its pattern be stratiform, including water chestnut square structure α-
Fe2O3With the FeVO of three monoclinic phases4.Present invention process is simple, easy to operate, and short preparation period, reaction condition are gentle, production efficiency
Height, target product structure and morphology controllable, and the α-Fe prepared2O3/FeVO4The photocatalysis performance of composite photo-catalyst is purer
Phase FeVO4It is more excellent, it can apply to degradation of organic substances under ultraviolet light.
The MODIFIED Fe VO provided in above-mentioned document4There is the spy higher to utilization rate of ultraviolet light mostly in composite photo-catalyst
Point, however, UV light only has 3%~5% sunshine, limits its practical application.Therefore, exploitation has good to visible ray
Response and the excellent photochemical catalyst of photocatalysis effect have broad prospects.
In recent years, MODIFIED Fe VO4Composite photo-catalyst in the existing relevant report such as photocatalysis degradation organic contaminant, but
The fluoroquinolone antibiotics such as Norfloxacin, Ciprofloxacin report is very few in Treatment by Photocatalysis Oxidation water.
The content of the invention
Present invention aims at propose a kind of C/Fe-FeVO4Composite photo-catalyst and its preparation method and application, to solve
Prepare FeVO4The undesirable problem of the visible light utilization efficiency of photochemical catalyst.
The present invention is with Fe (NO3)3·9H2O and NH4VO3For key reaction raw material, and using carbon paste ball as carrier, use water
Thermal synthesis method has synthesized visible under conditions of different temperatures, different pH value and different hydro-thermal times, different surfaces activating agent
The C/Fe-FeVO of photoresponse4Composite photo-catalyst, to expand C/Fe-FeVO4Promise fluorine in water removal is removed in photochemical catalyst photochemical catalytic oxidation
The research and development of the emerging micropollutants such as Sha Xing, Ciprofloxacin provides Technical Reference.
Above-mentioned purpose is realized, the technical scheme that the present invention takes is as follows：
A kind of C/Fe-FeVO4The preparation method of composite photo-catalyst, this method comprises the following steps：
Step 1: glucose, ferrous gluconate are mixed, add deionized water and stir to clarify and material is all molten
Solution, be placed in hydrothermal reaction kettle, 8h reacted under conditions of 160 DEG C, after taking out reactor after its natural cooling, spend successively from
Sub- water and absolute ethyl alcohol washing, and the sediment after washing is dried in vacuo, carrier carbon glueballs needed for obtaining；
Carry out ultrasonically treated Step 2: taking carbon paste ball made from step one to add into deionized water, afterwards, Fe is taken respectively
(NO3)3·9H2O、NH4VO3With SDBS surfactants, add after being mixed in described carbon paste ball, proceed it is ultrasonically treated,
Then stir to being sufficiently mixed, use 2mol/LHNO3Or 1mol/LNaOH adjusts the pH value of solution again, grey solution is obtained, then
Magnetic agitation is carried out again, makes solution reaction complete；
Step 3: the stainless steel cauldron for complete grey solution will be reacted in step 2 being positioned over polytetrafluoroethyllining lining
In, reacted under hydrothermal conditions, be cooled to room temperature, obtain turbid solution；
Step 4: the turbid solution obtained by step 3 is centrifuged, washed respectively with water and ethanol, Ran Hougan
It is dry, that is, obtain C/Fe-FeVO4Presoma；
Step 5: by the C/Fe-FeVO obtained by step 44Presoma is calcined 2-4h under the conditions of 300-600 DEG C, is situated between
The C/Fe-FeVO of hole flaky nanometer structure composition4。
A kind of C/Fe-FeVO4The preparation method of composite photo-catalyst obtains C/Fe-FeVO4Composite photo-catalyst, mainly by C
Element, Fe elements, O elements and V element composition, C/Fe-FeVO4Composite photo-catalyst is a kind of meso-porous nano laminated structure.
A kind of C/Fe-FeVO4C/Fe-FeVO made from the preparation method of composite photo-catalyst4Composite photo-catalyst is visible
Ciprofloxacin, the application of the emerging micropollutants of Norfloxacin are handled under light.
The present invention is relative to the beneficial effect of prior art：
(1) C/Fe-FeVO of the meso-porous nano piece composition obtained by4The micro-nano knot being made up of mesoporous nanometer sheet
Structure, with good dispersion, the advantages of not reuniting.
(2) C/Fe-FeVO of the meso-porous nano piece composition obtained by4Purity is high, does not contain the C/Fe- of other patterns
FeVO4。
(3) C/Fe-FeVO of the meso-porous nano piece composition obtained by4Performance is stable, in atmosphere not mutability.
(4) technique is simple, low for equipment requirements, raw material be easy to get to, it is low-cost, can be produced in enormous quantities.
(5) present invention provides efficient with good visible light-responded photochemical catalyst C/Fe-FeVO4, C/Fe modifications are not
But embryonic stem-like cells can be carried out by improving the iron ion in visible absorption, and C/Fe, so as to improve to Ciprofloxacin
Removal efficiency (as shown in Figure 5).
The C/Fe-FeVO of meso-porous nano laminated structure composition prepared by the present invention4Be conducive to opening up C/Fe-FeVO4Itself is solely
Special performance and application.
Brief description of the drawings
Fig. 1 is a kind of C/Fe-FeVO of the invention4The flow chart of the preparation method of composite photo-catalyst；
The C/Fe-FeVO that Fig. 2 constitutes for the meso-porous nano laminated structure in embodiment 14Stereoscan photograph；
The C/Fe-FeVO that Fig. 3 constitutes for the meso-porous nano laminated structure in embodiment 24Stereoscan photograph；
The C/Fe-FeVO that Fig. 4 constitutes for the meso-porous nano laminated structure in embodiment 34Stereoscan photograph；
The C/Fe-FeVO that Fig. 5 constitutes for the meso-porous nano laminated structure in embodiment 14UV-Vis DRS spectrum
(DRS) figure.
Technical scheme is further described below in conjunction with the accompanying drawings, but is not limited thereto, it is every to this
Inventive technique scheme is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, all should be covered
In protection scope of the present invention.
Embodiment
Embodiment one：As shown in figure 1, present embodiment discloses a kind of C/Fe-FeVO4Composite photo-catalyst
Preparation method, this method comprises the following steps：
Step 1: glucose, ferrous gluconate are mixed, add deionized water and stir to clarify and material is all molten
Solution, be placed in hydrothermal reaction kettle, 8h reacted under conditions of 160 DEG C, after taking out reactor after its natural cooling, spend successively from
Sub- water and absolute ethyl alcohol washing, and the sediment after washing is dried in vacuo, carrier carbon glueballs needed for obtaining；
Carry out ultrasonically treated Step 2: taking carbon paste ball made from step one to add into deionized water, afterwards, Fe is taken respectively
(NO3)3·9H2O、NH4VO3With SDBS surfactants, add after being mixed in described carbon paste ball, proceed it is ultrasonically treated,
Then stir to being sufficiently mixed, use 2mol/LHNO3Or 1mol/LNaOH adjusts the pH value of solution again, grey solution is obtained, then
Magnetic agitation is carried out again, makes solution reaction complete；
Step 3: the stainless steel cauldron for complete grey solution will be reacted in step 2 being positioned over polytetrafluoroethyllining lining
In, reacted under hydrothermal conditions, be cooled to room temperature, obtain turbid solution；
Step 4: the turbid solution obtained by step 3 is centrifuged, washed respectively with water and ethanol, Ran Hougan
It is dry, that is, obtain C/Fe-FeVO4Presoma；
Step 5: by the C/Fe-FeVO obtained by step 44Presoma is calcined 2-4h under the conditions of 300-600 DEG C, is situated between
The C/Fe-FeVO of hole flaky nanometer structure composition4。
Embodiment two：Present embodiment be to further illustrating that embodiment one is made, in step one,
It is 1 in mass ratio by described glucose and ferrous gluconate:0.6 ratio mixing, adds deionized water and stirs to clarify
And all dissolve material, the proportioning of glucose and deionized water is (0.4-1g)：(40-100mL), after described washing
Sediment is dried in vacuo 4h at a temperature of being placed on 40 °.
Present embodiment is mainly judged according to the height of the photocatalytic degradation effects such as photochemical catalytic oxidation Ciprofloxacin
, on this condition, there is higher clearance to Ciprofloxacin.
Embodiment three：Present embodiment be to further illustrating that embodiment one is made, in step 2,
Described carbon paste ball and the proportioning of deionized water are (0.4-1) g：(40-100) mL, sonication treatment time is 10min, is taken respectively
Fe(NO3)3·9H2O、NH4VO3With SDBS surfactants, add after being mixed in described carbon paste ball, proceed ultrasonically treated
Time be 10min, use 2mol/LHNO3Or 1mol/LNaOH adjusts the pH=3 of solution.
Embodiment four：Present embodiment be to further illustrating that embodiment three is made, in step 2,
Described Fe (NO3)3·9H2O and NH4VO3Mass ratio be 10:3；Fe(NO3)3·9H2O and SDBS proportioning is 0.4g：
(0.15-0.3)g；
Embodiment five：Present embodiment be to further illustrating that embodiment one is made, in step 3,
Reaction 12-30h is carried out under 120-200 DEG C of hydrothermal condition.Present embodiment is mainly according to photochemical catalytic oxidation Ciprofloxacin etc.
What the height of photocatalytic degradation effect was judged, on this condition, there is higher clearance to Ciprofloxacin.
Embodiment six：A kind of C/Fe-FeVO in embodiment one to five described in any embodiment4Complex light
The preparation method of catalyst obtains C/Fe-FeVO4Composite photo-catalyst, mainly by C element, Fe elements, O elements and V element group
Into C/Fe-FeVO4Composite photo-catalyst is a kind of meso-porous nano laminated structure.
Embodiment seven：A kind of C/Fe-FeVO in embodiment one to five described in any embodiment4Complex light
C/Fe-FeVO made from the preparation method of catalyst4It is new that composite photo-catalyst handles Ciprofloxacin, Norfloxacin under visible light
The application of emerging micropollutants.
Embodiment 1
This embodiment discloses herein a kind of C/Fe-FeVO4The preparation method of composite photo-catalyst, described preparation method step
As follows (referring to Fig. 1)；
Make its abundant Step 1: 4.0g glucose and 2.4g ferrous gluconates are dissolved in into ultrasound in 40mL water, stirring
Dissolving；Mixed solution is positioned in the stainless steel cauldron of polytetrafluoroethyllining lining, sealing is reacted under conditions of 160 DEG C
8h, is cooled to room temperature, obtains turbid solution and is centrifuged, and is washed, is then dried respectively with water and ethanol, produces carbon paste ball；
Ultrasound in 40mL water, stirring are dissolved in Step 2: weighing and carbon paste ball 0.4g being made in step one, is then respectively adding
The SDBS of 0.4g ferric nitrates, 0.12g ammonium metavanadates and 0.15g, uses 2mol/LHNO3Or 1mol/LNaOH adjusts the pH=of solution
3, stir 30min；
Step 3: the mixed solution of step 2 is positioned in the stainless steel cauldron of polytetrafluoroethyllining lining, after sealing
24h is reacted under conditions of 180 DEG C, is cooled to after room temperature, turbid solution is obtained；
Step 4: turbid solution obtained by step 3 is centrifuged, washed, then dried respectively with water and ethanol,
Produce C/Fe-FeVO4Presoma；
Step 5: by C/Fe-FeVO4Presoma is calcined 2h under the conditions of 500 DEG C, obtains meso-porous nano laminated structure composition
C/Fe-FeVO4。
Advantage of this embodiment is that：The present embodiment is mainly according to photocatalytic degradation effects such as photochemical catalytic oxidation Ciprofloxacins
Height judged on this condition, there is higher clearance to Ciprofloxacin, pattern preferably, as shown in Figure 2.
Embodiment 2
This embodiment discloses herein a kind of C/Fe-FeVO4The preparation method of composite photo-catalyst, described preparation method step
As follows (referring to Fig. 1)；
Make its abundant Step 1: 4.0g glucose and 2.4g ferrous gluconates are dissolved in into ultrasound in 40mL water, stirring
Dissolving；Mixed solution is positioned in the stainless steel cauldron of polytetrafluoroethyllining lining, sealing is reacted under conditions of 160 DEG C
8h, is cooled to room temperature, obtains turbid solution and is centrifuged, and is washed, is then dried respectively with water and ethanol, produces carbon paste ball；
Ultrasound in 40mL water, stirring are dissolved in Step 2: weighing and carbon paste ball 0.4g being made in step one, is then respectively adding
The SDBS of 0.4g ferric nitrates, 0.12g ammonium metavanadates and 0.3g, uses 2mol/LHNO3Or 1mol/LNaOH adjusts the pH=3 of solution,
Stir 30min；
Step 3: the mixed solution of step 2 is positioned in the stainless steel cauldron of polytetrafluoroethyllining lining, after sealing
24h is reacted under conditions of 180 DEG C, is cooled to after room temperature, turbid solution is obtained；
Step 4: turbid solution obtained by step 3 is centrifuged, washed, then dried respectively with water and ethanol,
Produce C/Fe-FeVO4Presoma；
Step 5: by C/Fe-FeVO4Presoma is calcined 2h under the conditions of 600 DEG C, obtains meso-porous nano laminated structure composition
C/Fe-FeVO4。
The advantage or effect of the present embodiment be：Mainly according to photocatalytic degradation effects such as photochemical catalytic oxidation Ciprofloxacins
What height was judged, on this condition, there is higher clearance to Ciprofloxacin, but pattern is slightly worse as shown in Figure 3.
Embodiment 3
This embodiment discloses herein a kind of C/Fe-FeVO4The preparation method of composite photo-catalyst, described preparation method step
As follows (referring to Fig. 1)；
Make its abundant Step 1: 4.0g glucose and 2.4g ferrous gluconates are dissolved in into ultrasound in 40mL water, stirring
Dissolving；Mixed solution is positioned in the stainless steel cauldron of polytetrafluoroethyllining lining, sealing is reacted under conditions of 160 DEG C
8h, is cooled to room temperature, obtains turbid solution and is centrifuged, and is washed, is then dried respectively with water and ethanol, produces carbon paste ball；
Ultrasound in 40mL water, stirring are dissolved in Step 2: weighing and carbon paste ball 0.4g being made in step one, is then respectively adding
The SDBS of 0.4g ferric nitrates, 0.12g ammonium metavanadates and 0.15g, uses 2mol/LHNO3Or 1mol/LNaOH adjusts the pH=of solution
3, stir 30min；
Step 3: the mixed solution of step 2 is positioned in the stainless steel cauldron of polytetrafluoroethyllining lining, after sealing
24h is reacted under conditions of 120 DEG C, is cooled to after room temperature, turbid solution is obtained；
Step 4: turbid solution obtained by step 3 is centrifuged, washed, then dried respectively with water and ethanol,
Produce C/Fe-FeVO4Presoma；
Step 5: by C/Fe-FeVO4Presoma is calcined 2h under the conditions of 300 DEG C, obtains meso-porous nano laminated structure composition
C/Fe-FeVO4。
The effect of the present embodiment is：Mainly entered according to the height of the photocatalytic degradation effects such as photochemical catalytic oxidation Ciprofloxacin
What row judged, on this condition, the clearance that Ciprofloxacin has is decreased, but pattern is poor, as shown in Figure 4.
Claims (7)
1. a kind of C/Fe-FeVO4The preparation method of composite photo-catalyst, it is characterised in that：This method comprises the following steps：
Step 1: glucose, ferrous gluconate are mixed, add deionized water and stir to clarify and all dissolve material,
It is placed in hydrothermal reaction kettle, 8h is reacted under conditions of 160 DEG C, after taking out reactor after its natural cooling, deionization is used successively
Water and absolute ethyl alcohol washing, and the sediment after washing is dried in vacuo, carrier carbon glueballs needed for obtaining；
Carry out ultrasonically treated Step 2: taking carbon paste ball made from step one to add into deionized water, afterwards, Fe is taken respectively
(NO3)3·9H2O、NH4VO3With SDBS surfactants, add after being mixed in described carbon paste ball, proceed it is ultrasonically treated,
Then stir to being sufficiently mixed, use 2mol/LHNO3Or 1mol/LNaOH adjusts the pH value of solution again, grey solution is obtained, then
Magnetic agitation is carried out again, makes solution reaction complete；
Step 3: be positioned over complete grey solution is reacted in step 2 in the stainless steel cauldron of polytetrafluoroethyllining lining,
Reacted under hydrothermal conditions, be cooled to room temperature, obtain turbid solution；
Step 4: the turbid solution obtained by step 3 is centrifuged, washed, then dried, i.e., respectively with water and ethanol
Obtain C/Fe-FeVO4Presoma；
Step 5: by the C/Fe-FeVO obtained by step 44Presoma is calcined 2-4h under the conditions of 300-600 DEG C, obtains mesoporous receive
The C/Fe-FeVO of rice laminated structure composition4。
2. a kind of C/Fe-FeVO according to claim 14The preparation method of composite photo-catalyst, it is characterised in that：Step
It is 1 in mass ratio by described glucose and ferrous gluconate in one:0.6 ratio mixing, add deionized water stir to
Clarify and all dissolve material, the proportioning of glucose and deionized water is (0.4-1g)：(40-100mL), by described washing
Sediment afterwards is dried in vacuo 4h at a temperature of being placed on 40 °.
3. a kind of C/Fe-FeVO according to claim 14The preparation method of composite photo-catalyst, it is characterised in that：Step
In two, described carbon paste ball and the proportioning of deionized water are (0.4-1) g：(40-100) mL, sonication treatment time is 10min, point
Fe (NO are not taken3)3·9H2O、NH4VO3With SDBS surfactants, add after being mixed in described carbon paste ball, proceed ultrasound
The time of processing is 10min, uses 2mol/LHNO3Or 1mol/LNaOH adjusts the pH=3 of solution.
4. a kind of C/Fe-FeVO according to claim 34The preparation method of composite photo-catalyst, it is characterised in that：Step
In two, described Fe (NO3)3·9H2O and NH4VO3Mass ratio be 10:3；Fe(NO3)3·9H2O and SDBS proportioning is
0.4g：(0.15-0.3)g.
5. a kind of C/Fe-FeVO according to claim 14The preparation method of composite photo-catalyst, it is characterised in that：Step
In three, reaction 12-30h is carried out under 120-200 DEG C of hydrothermal condition.
6. the C/Fe-FeVO in a kind of claim 1 to 5 described in any claim4The preparation method of composite photo-catalyst is obtained
C/Fe-FeVO4Composite photo-catalyst, it is characterised in that：Mainly it is made up of C element, Fe elements, O elements and V element, C/Fe-
FeVO4Composite photo-catalyst is a kind of meso-porous nano laminated structure.
7. the C/Fe-FeVO in a kind of claim 1 to 5 described in any claim4The preparation method of composite photo-catalyst is made
C/Fe-FeVO4Composite photo-catalyst handles the application of the emerging micropollutants of Ciprofloxacin, Norfloxacin under visible light.
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| CN113511688B (en) * | 2021-08-25 | 2023-05-26 | 杭州恒毅智创科技有限公司 | FeVO (FeVO) 4 Preparation method of hollow sphere |
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