CN106540703A - A kind of preparation method of Fe doping zinc oxide nanometers photocatalyst - Google Patents
A kind of preparation method of Fe doping zinc oxide nanometers photocatalyst Download PDFInfo
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- CN106540703A CN106540703A CN201611108460.1A CN201611108460A CN106540703A CN 106540703 A CN106540703 A CN 106540703A CN 201611108460 A CN201611108460 A CN 201611108460A CN 106540703 A CN106540703 A CN 106540703A
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- 238000001556 precipitation Methods 0.000 claims abstract description 44
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 34
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000011701 zinc Substances 0.000 claims abstract description 22
- 230000001699 photocatalysis Effects 0.000 claims abstract description 20
- 238000007146 photocatalysis Methods 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 239000002351 wastewater Substances 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 7
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052753 mercury Inorganic materials 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 238000002835 absorbance Methods 0.000 claims description 2
- 238000000862 absorption spectrum Methods 0.000 claims description 2
- 238000011056 performance test Methods 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 33
- 229910002596 FexO Inorganic materials 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 abstract description 4
- 239000011943 nanocatalyst Substances 0.000 abstract description 2
- 125000000636 p-nitrophenyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)[N+]([O-])=O 0.000 abstract description 2
- 239000011592 zinc chloride Substances 0.000 abstract description 2
- 235000005074 zinc chloride Nutrition 0.000 abstract description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000006065 biodegradation reaction Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- -1 Iron ion Chemical class 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000013461 intermediate chemical Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000009377 nuclear transmutation Methods 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—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
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
A kind of preparation method of Fe doping zinc oxide nanometers photocatalyst, is related to a kind of preparation method of catalyst, and the present invention prepares Zn using sluggish precipitation by raw material of Iron(III) chloride hexahydrate, zinc chloride, citric acid and sodium hydroxide under room temperature open system1‑xFexO photocatalysts.With fluorescent high-pressure mercury lamp as light source, to make Zn by oneself1‑ xFexO is catalyst, and p-nitrophenyl waste water carries out photocatalysis treatment, and the photocatalysis performance of catalyst is investigated with the clearance of nitrobenzene waste water.With Zn1‑xFexO is catalyst, is entrained in ZnO by Fe and introduces doped energy-band, has expanded the photoresponse scope of ZnO nano catalyst, and then has obtained good catalytic efficiency.Under the irradiation of 125W fluorescent high-pressure mercury lamps, work as nFe:nZnFor 1:99、n(Fe+Zn):nCitric acidFor 1:3rd, concentration of sodium hydroxide solution be 0.4mol/L, calcining heat be 500 DEG C, nZn1‑xFexO:nNitrobenzolFor 2:1st, when sample time is 3h, the clearance of nitrobenzene waste water reaches more than 70%.
Description
Technical field
The present invention relates to a kind of preparation method of catalyst, more particularly to a kind of Fe doping zinc oxide nanometers photocatalyst
Preparation method.
Background technology
Water is most important living matter for the survival of mankind.Either drink, agricultural irrigation or water for industrial use, all
There is substantial amounts of demand to water.However, with the fast development of global industry, discharge of industrial wastes is more and more, the pollution to water source
Also it is increasingly severe so that the environment that people depend on for existence receives serious threat.Wherein Nitrobenzol (Nitrobenzene,
NB) as Organic Chemical Industry in a kind of important fine-chemical intermediate and industrial chemicals, be widely used in recent years simultaneously
It is discharged in environment, Long Term Contact, it is very harmful to human body and animals and plants, serious problem of environmental pollution is caused, its pollution is useless
Water has been listed in priority pollutants.Therefore, the improvement of p-nitrophenyl waste water has become people's problem in the urgent need to address.
Main processing method has：Biodegradation, physical absorption and chemical oxidative decomposition etc..And biodegradation easily cause transmutation of species and
Easily there is parsing problem in the problems such as destruction ecological balance, physical absorption, thus method the most effective is using chemistry side
Method is decomposing organic pollutants.Therefore, by the use of semiconductor nano material as photocatalyst, catalytic degradation organic contamination is given up
Water, it is widely studied by environment scholar both domestic and external as a kind of effective method curbed environmental pollution.
Currently, in the world can be numerous as the material of photocatalyst, including TiO2、ZnO、ZrO2Partly lead Deng many oxide
Body, wherein TiO2Because its oxidability is strong, stable chemical nature is nontoxic, becomes most widely used nano-photo catalytic material in the world
Material.But due to TiO2Light induced electron and photohole easily compound, visible light photocatalysis efficiency are there is in photocatalytic process
The shortcomings of relatively low, high energy consumption, crystal formation are variable, greatly constrains TiO2As the practical application of photocatalyst.And nano-ZnO by
Have and TiO in which2Close energy gap, and it is excellent with simple and direct, cheap, efficient, nontoxic and stable crystal form etc. is prepared
Point is considered as one of high-activity photocatalyst of great application prospect of alternative titanium dioxide, in recent years with regard to its preparation
And its performance study has become the focus in catalyticing research field, and extensively applied.
At present, for the research of ZnO catalysis materials focuses principally on the raising of photocatalysis efficiency and photoresponse scope
In terms of widening the two.It is well known that the energy gap of ZnO is 3.37eV, thus photoresponse scope is in ultraviolet region, to visible
The utilization rate of light and infrared light district is low.UV energy less than 400nm or so probably only accounts for the 4% of solar energy, how to utilize
Visible ray or even infrared energy, are to determine that can catalysis material be able to the prerequisite of large-scale practical application.Therefore will
Iron ion is incorporated in ZnO lattices, forms the impurity energy level of defect level or localized state, and introduce what is enriched in its band gap
Lacking oxygen, can reach the purpose that photo-generated carrier is efficiently separated while ZnO photoresponse scopes are widened.
The preparation method of Fe doping zinc oxide nanometer photocatalysts mainly includes:Chemical precipitation method, hydrothermal synthesis method, colloidal sol are coagulated
Glue method, sluggish precipitation, solid-phase synthesis, microemulsion method etc..But it is multiple that technique is still suffered from the preparation method of nano zine oxide
The shortcomings of serious, particle bad dispersibility that miscellaneous, industrialization difficulty is big, nano zine oxide is reunited.Therefore exploitation is simple efficiently, be easy to work
The emphasis of research is produced, become with good dispersion, the nano zinc oxide material that energy consumption is low, photocatalytic activity is high to industry metaplasia.This
It is bright to relate to a kind of co-precipitation preparation method of Fe doping zinc oxide nanometers catalyst, it is entrained in ZnO by Fe and introduces doping energy
Level, has expanded the photoresponse scope of ZnO nano catalyst, and then has obtained good catalytic efficiency.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Fe doping zinc oxide nanometers photocatalyst, the present invention is with six water
Conjunction ferric chloride and zinc chloride prepare the Zn of non-secondary pollution energy recycling for material1-xFexO catalyst materials, it is determined that
Zn1-xFexThe optimal preparation method of O catalyst materials, the photocatalysis performance to improve catalyst itself provide technological guidance and Li
By support.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of Fe doping zinc oxide nanometers photocatalyst, methods described include procedure below：
1. 100mL ZnCl are separately added in 1000mL beakers2And FeCl3Mixed solution and 100mL citric acid solutions, magnetic
Power stirs 1h, is allowed to mix homogeneously；Under stirring, sodium hydroxide solution, adition process are added dropwise over toward above-mentioned mixed liquor
In have Precipitation, when precipitation disappear, stop Deca sodium hydroxide solution；Stand, have Precipitation.Gained precipitation is distilled
Water cleaning is until cleanout fluid is bordering on neutrality；
2. the precipitation after cleaning is put in 80 DEG C of drying baker and is dried, to constant weight；
3. the precipitation after drying is put in agate mortar and is ground, the powder after grinding is put in crucible, Muffle furnace is placed in
Middle calcining 2h.After end, take out, it is standby；
4. photocatalysis performance test is carried out using nitrobenzene waste water：The catalyst for having prepared is taken, 300mL is added to, concentration is
In the nitrobenzene solution of 400mg/L, stir, dark place stands 1h.Above-mentioned sample several pieces are taken, 125W fluorescent high-pressure mercury lamps are used
Irradiate simultaneously, react the absorption spectrum of sampling and measuring nitrobenzene waste water after 3h, device therefor is the UV-2550 of Japanese Shimadzu Corporation
Type ultra-violet and visible spectrophotometer；Using the absorbance of ultraviolet-uisible spectrophotometer measuring samples at the wavelength 267nm,
Return the initial mass concentration of NitrobenzolWith concentration after degraded, and calculate clearance；
（1）；
Formula（1）In,- Nitrobenzol initial mass concentration, mg/L；The concentration of solution, mg/L after-degraded.
A kind of preparation method of described Fe doping zinc oxide nanometers photocatalyst, the nFe 3+:nZn 2+For 1:99.
A kind of preparation method of described Fe doping zinc oxide nanometers photocatalyst, the n(Fe 3+ +Zn 2+ ):nCitric acidFor 1:3.
A kind of preparation method of described Fe doping zinc oxide nanometers photocatalyst, the concentration of sodium hydroxide solution is
0.4mol/L。
A kind of preparation method of described Fe doping zinc oxide nanometers photocatalyst, the calcining heat are 500 DEG C.
A kind of preparation method of described Fe doping zinc oxide nanometers photocatalyst, the mZn0.99Fe0.01O:mNitrobenzolFor 2:1.
Advantages of the present invention with effect is：
With fluorescent high-pressure mercury lamp as light source, to make Zn1-xFexO by oneself as catalyst, photocatalysis treatment nitrobenzene waste water has the present invention
Have the advantages that non-secondary pollution, cheap, good mechanical property, method are simple, quick.
（1）Adulterate in ZnO after Fe, spectral absorption scope is widened, light source utilization rate is improved；
（2）After Fe doping, catalyst is made per se with magnetic, beneficial to the recycling of catalyst；
（3）It is radiation energy using the ultraviolet light of non-secondary pollution and low energy consumption, meets environmental protection with resource-conserving country
Build, and solve the resource problem of China's water quality hydropenia.
Description of the drawings
Fig. 1 is the process chart for synthesizing Fe dopen Nano ZnO catalyst powder.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
Embodiment 1nFe 3+With nZn 2+Impact of the ratio to photocatalysis performance
At ambient temperature, to 100mL Zn2+And Fe3+Total concentration is 0.1mol/L, nFe 3+:nZn 2+Respectively 0/100,0.5/
99.5th, it is 0.3 mol/L citric acid solutions that 1/99,2/98,5/95 mixed solution adds 100mL concentration, stirs 1h, is allowed to mixed
Close uniform.It is 0.4mol/L sodium hydroxide solutions to be added dropwise over concentration afterwards, has Precipitation, when precipitation disappears during being added dropwise to
Lose, stop Deca sodium hydroxide solution.Stand, have Precipitation.Gained precipitation is cleaned with distilled water until cleanout fluid is bordering on
It is neutral.Precipitation after cleaning is put in 80 DEG C of drying baker and is dried, to constant weight, the precipitation after drying is put into into agate mortar then
Middle grinding, the powder after grinding is put in crucible, calcines 2h in being placed in 400 DEG C of Muffle furnaces.After end, take out, it is standby.
The test of photocatalysis performance, with 125W fluorescent high-pressure mercury lamps as light source, to 300mL, nitro of the concentration for 400mg/L
The Zn of 0.12g is added in benzole soln1-xFexO, response time are 3h.Work as nFe 3+:nZn 2+For 1/99 when, the removal effect of Nitrobenzol
Preferably, clearance is 54.8%.
2 n of embodiment(Fe 3+ +Zn 2+ )With nCitric acidImpact of the ratio to photocatalysis performance
At ambient temperature, to 100mL Zn2+And Fe3+Total concentration is 0.1mol/L, nFe 3+:nZn 2+For 1/99 mixed solution
100mL concentration is added to be respectively 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L citric acid molten
Liquid, stirs 1h, is allowed to mix homogeneously.It is 0.4mol/L sodium hydroxide solutions to be added dropwise over concentration afterwards, is had during being added dropwise to
Precipitation, when precipitation disappears, stops Deca sodium hydroxide solution.Stand, have Precipitation.Will be gained precipitation clear with distilled water
Wash until cleanout fluid is bordering on neutrality.Precipitation after cleaning is put in 80 DEG C of drying baker and is dried, to constant weight, then by after drying
Precipitation is ground in being put into agate mortar, and the powder after grinding is put in crucible, 2h is calcined in being placed in 400 DEG C of Muffle furnaces.Knot
Shu Hou, takes out, standby.
The test of photocatalysis performance is carried out according to the experimentation in embodiment 1.Work as n(Fe 3+ +Zn 2+ ):nCitric acidFor 1:When 3, nitre
Preferably, clearance is 55.2% to the removal effect of base benzene.
Impact of 3 concentration of sodium hydroxide solution of embodiment to photocatalysis performance
At ambient temperature, to 100mL Zn2+And Fe3+Total concentration is 0.1mol/L, nFe 3+:nZn 2+For 1/99 mixed solution
Add 100mL concentration to be 0.3mol/L citric acid solutions, stir 1h, be allowed to mix homogeneously.It is added dropwise over concentration afterwards to be respectively
0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L sodium hydroxide solution, has precipitation analysis during being added dropwise to
Go out, when precipitation disappears, stop Deca sodium hydroxide solution.Stand, have Precipitation.Gained precipitation is cleaned with distilled water until
Cleanout fluid is bordering on neutrality.Precipitation after cleaning is put in 80 DEG C of drying baker and is dried, to constant weight, then the precipitation after drying is put
Grind in entering agate mortar, the powder after grinding is put in crucible, in being placed in 400 DEG C of Muffle furnaces, 2h is calcined.After end, take
Go out, it is standby.
The test of photocatalysis performance is carried out according to the experimentation in embodiment 1.When concentration of sodium hydroxide solution is
During 0.4mol/L, preferably, clearance is 55.3% to the removal effect of Nitrobenzol.
Impact of the 4 catalyst calcination temperature of embodiment to photocatalysis performance
At ambient temperature, to 100mL Zn2+And Fe3+Total concentration is 0.1mol/L, nFe 3+:nZn 2+For 1/99 mixed solution
Add 100mL concentration to be 0.3mol/L citric acid solutions, stir 1h, be allowed to mix homogeneously.It is added dropwise over concentration afterwards to be respectively
0.4mol/L sodium hydroxide solutions, have Precipitation during being added dropwise to, when precipitation disappears, stop Deca sodium hydroxide solution.
Stand, have Precipitation.Gained precipitation is cleaned with distilled water until cleanout fluid is bordering on neutrality.Precipitation after cleaning is put into into 80
Dry in DEG C drying baker, to constant weight, then the precipitation after drying is put in agate mortar and is ground, the powder after grinding is put into
In crucible, and be respectively placed in 400 DEG C, 500 DEG C, calcine 2h in 600 DEG C of Muffle furnaces.After end, take out, it is standby.
The test of photocatalysis performance is carried out according to the experimentation in embodiment 1.When calcining heat is 500 DEG C, nitro
Preferably, clearance is 65.6% to the removal effect of benzene.
5 m of embodimentZn0.99Fe0.01OWith mNitrobenzolFor 2:Impact of 1 ratio to photocatalysis performance
At ambient temperature, to 100mL Zn2+And Fe3+Total concentration is 0.1mol/L, nFe 3+:nZn 2+For 1/99 mixed solution
Add 100mL concentration to be 0.3mol/L citric acid solutions, stir 1h, be allowed to mix homogeneously.It is added dropwise over concentration afterwards to be respectively
0.4mol/L sodium hydroxide solutions, have Precipitation during being added dropwise to, when precipitation disappears, stop Deca sodium hydroxide solution.
Stand, have Precipitation.Gained precipitation is cleaned with distilled water until cleanout fluid is bordering on neutrality.Precipitation after cleaning is put into into 80
Dry in DEG C drying baker, to constant weight, then the precipitation after drying is put in agate mortar and is ground, the powder after grinding is put into
In crucible, and 2h is calcined in being respectively placed in 500 DEG C of Muffle furnaces.After end, take out, it is standby.
The test of photocatalysis performance, with 125W fluorescent high-pressure mercury lamps as light source, to 300mL, nitro of the concentration for 400mg/L
The Zn of 0.06g, 0.12g, 0.24g, 0.36g, 0.48g is separately added in benzole soln0.99Fe0.01O, response time are 3h.When
mZn0.99Fe0.01O:mNitrobenzolFor 2:When 1, preferably, clearance is 75.6% to the removal effect of Nitrobenzol.
Above content is the further description done to the present invention with reference to optimal technical scheme, it is impossible to assert the present invention's
It is embodied as being only limitted to these explanations.For general technical staff of the technical field of the invention, without departing from the present invention
Design on the premise of made change, modification, replacement, combination, simplify, should be equivalent substitute mode, should all be considered as
Protection scope of the present invention.
Claims (6)
1. a kind of preparation method of Fe doping zinc oxide nanometers photocatalyst, it is characterised in that methods described includes procedure below：
1. 100mL ZnCl are separately added in 1000mL beakers2And FeCl3Mixed solution and 100mL citric acid solutions, magnetic
Power stirs 1h, is allowed to mix homogeneously；Under stirring, sodium hydroxide solution, adition process are added dropwise over toward above-mentioned mixed liquor
In have Precipitation, when precipitation disappear, stop Deca sodium hydroxide solution；Stand, have Precipitation；
Gained precipitation is cleaned with distilled water until cleanout fluid is bordering on neutrality；
2. the precipitation after cleaning is put in 80 DEG C of drying baker and is dried, to constant weight；
3. the precipitation after drying is put in agate mortar and is ground, the powder after grinding is put in crucible, Muffle furnace is placed in
Middle calcining 2h；
After end, take out, it is standby；
4. photocatalysis performance test is carried out using nitrobenzene waste water：The catalyst for having prepared is taken, 300mL is added to, concentration is
In the nitrobenzene solution of 400mg/L, stir, dark place stands 1h；
Above-mentioned sample several pieces are taken, is irradiated with 125W fluorescent high-pressure mercury lamps simultaneously, sampling and measuring nitrobenzene waste water after reaction 3h
Absorption spectrum, device therefor are the UV-2550 type ultra-violet and visible spectrophotometers of Japanese Shimadzu Corporation；Using UV, visible light point
The absorbance of light photometer measuring samples at the wavelength 267nm, returns the initial mass concentration of NitrobenzolIt is dense with after degraded
Degree, and calculate clearance；
（1）；
Formula（1）In,- Nitrobenzol initial mass concentration, mg/L；The concentration of solution, mg/L after-degraded.
2. the preparation method of a kind of Fe doping zinc oxide nanometers photocatalyst according to claim 1, it is characterised in that described
nFe 3+:nZn 2+For 1:99.
3. the preparation method of a kind of Fe doping zinc oxide nanometers photocatalyst according to claim 1, it is characterised in that described
n(Fe 3+ +Zn 2+ ):nCitric acidFor 1:3.
4. the preparation method of a kind of Fe doping zinc oxide nanometers photocatalyst according to claim 1, it is characterised in that described
Concentration of sodium hydroxide solution is 0.4mol/L.
5. the preparation method of a kind of Fe doping zinc oxide nanometers photocatalyst according to claim 1, it is characterised in that described
Calcining heat is 500 DEG C.
6. the preparation method of a kind of Fe doping zinc oxide nanometers photocatalyst according to claim 1, it is characterised in that described
mZn0.99Fe0.01O:mNitrobenzolFor 2:1.
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