CN108393089A - A kind of loess loading nanometer Fe nton photochemical catalysts and preparation method thereof - Google Patents
A kind of loess loading nanometer Fe nton photochemical catalysts and preparation method thereof Download PDFInfo
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- CN108393089A CN108393089A CN201810348467.3A CN201810348467A CN108393089A CN 108393089 A CN108393089 A CN 108393089A CN 201810348467 A CN201810348467 A CN 201810348467A CN 108393089 A CN108393089 A CN 108393089A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 55
- 238000011068 loading method Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000012153 distilled water Substances 0.000 claims abstract description 18
- 239000000725 suspension Substances 0.000 claims abstract description 15
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 6
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 4
- 230000008021 deposition Effects 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 230000020477 pH reduction Effects 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 8
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000010919 dye waste Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 49
- 230000015556 catabolic process Effects 0.000 description 10
- 238000006731 degradation reaction Methods 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- JUQPZRLQQYSMEQ-UHFFFAOYSA-N CI Basic red 9 Chemical compound [Cl-].C1=CC(N)=CC=C1C(C=1C=CC(N)=CC=1)=C1C=CC(=[NH2+])C=C1 JUQPZRLQQYSMEQ-UHFFFAOYSA-N 0.000 description 8
- 229940052223 basic fuchsin Drugs 0.000 description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 3
- 238000009303 advanced oxidation process reaction Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- -1 hydroxyl radical free radical Chemical class 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- SRUWWOSWHXIIIA-UKPGNTDSSA-N Cyanoginosin Chemical compound N1C(=O)[C@H](CCCN=C(N)N)NC(=O)[C@@H](C)[C@H](C(O)=O)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](C)NC(=O)C(=C)N(C)C(=O)CC[C@H](C(O)=O)N(C)C(=O)[C@@H](C)[C@@H]1\C=C\C(\C)=C\[C@H](C)[C@@H](O)CC1=CC=CC=C1 SRUWWOSWHXIIIA-UKPGNTDSSA-N 0.000 description 1
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 229910001919 chlorite Inorganic materials 0.000 description 1
- 229910052619 chlorite group Inorganic materials 0.000 description 1
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 238000007172 homogeneous catalysis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 108010067094 microcystin Proteins 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012916 structural analysis Methods 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
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/39—
-
- 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
- C02F1/722—Oxidation by peroxides
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation method of loess loading nanometer Fe nton photochemical catalysts, be by loess it is acidified after be scattered in distilled water loess suspension be made；Under inert gas protection, ferrous sulfate solution is added in loess suspension, after being stirred at room temperature, reducing agent is added and continues to be stirred to react；Deposition is stood after reaction, after gained deposit is washed repeatedly with distilled water, is dried in vacuo to get black powder loess loading nanometer Fe nton photochemical catalysts.Photocatalytic Degradation Property test shows, loess loading nanometer Fe nton photochemical catalysts prepared by the present invention have good photocatalytic activity under the irradiation of visible light, and the photochemical catalyst have the characteristics that raw material be easy to get, be of low cost, eco-friendly, photocatalytic degradation of dye waste water field have good application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of loess loading nanometer Fe nton photochemical catalysts, belong to field of compound material and
Technical field of waste water processing.
Background technology
Nearly recent decades, with a large amount of uses of the high speed development and fossil resources of modern industry, environmental pollution becomes prestige
Coerce the outstanding problem of human lives, wherein the organic pollution in waste water is a kind of important nuisance.There are many technologies
It is most popular at present to have absorption method, direct oxidation method, advanced oxidation processes applied to the removal of Organic Pollutants in Wastewater
Deng.Compared with traditional absorption method and direct oxidation method, advanced oxidation processes due to can by pollutant it is degradable be harmless CO2
And H2O, and have the advantages that non-secondary pollution, catalyst can recycle etc. and meet instantly environmentally protective and show more
Good application prospect.Advanced oxidation processes include Fenton methods, electrochemical process, ultrasonic oxidation method, photocatalytic oxidation and ozone oxygen
Change etc..
Fenton reactions are a kind of minimum high-level oxidation technologies of cost, have reaction unit is simple, reaction condition is mild,
The advantages such as operation cost is low, are concerned in the process field of organic wastewater.Traditional Fenton reactions are generally referred to as H2O2With
Fe2+The homogeneous catalysis system of composition, the disadvantage is that being difficult to detach after catalysis reaction, Fe2+Easy spilling leads to secondary pollution, and
And H2O2Consumption is larger, increases the cost of wastewater treatment.Heterogeneous Fenton catalysis is to utilize active particle component, i.e. handle
Fe0、Fe2+Or Fe3+It is carried on natural material（Such as carbon material, molecular sieve, clay class）, by H2O2It is converted into hydroxyl radical free radical
（•OH）To complete the degradation of organic pollution, it can be achieved that separation and recycling to solid catalyst.Utilize these carrier sheets
The absorption property that body has, further increases the catalytic efficiency of Fenton catalyst, while reducing cost.Such as：Wang Ying etc.（It is non-equal
Phase electro-fenton process handles waste water from dyestuff, contemporary chemical industry, 2015,44 (6): 1216-1218.）It is to urge with iron modified alta-mud
Agent, it is red using Fenton oxidative degradation dye activity, it is found that active red degradation rate reaches 98% or more.Huan Liang etc.
（J. Taiwan Inst. Chem. Eng., 2015, 49: 105-112）By Fe2O3It is carried on diatomite, and in light
Rhodamine B degradation under the conditions of Fenton finds that visible light can promote the generation of hydroxyl radical free radical, and degradation rate is up to 95%.Huang Yingping
Deng（CN 200910272152.6）It is prepared for heterophase Fenton photochemical catalyst by carrier of NaY molecular sieve, finds consolidating after load
Phase catalyst reaches 96% or so in 16 h to the degradation rate of Microcystin solution.Yu Xiaodan etc.（CN 107159211A）System
For Fe3O4/TiO2Composite material, nanometer Fe obtained3O4/TiO2Composite material has good chemical stability.In short, being
Keep the catalyst cost of preparation cheaper, application is more extensive, needs to find more cheap and effective carrier material.
Loess be it is a kind of derive from a wealth of sources, be nontoxic, non-secondary pollution, green natural inorganic silicate material cheap and easy to get.
Its loose lamellar structure makes it have certain adsorption capacity, acidified modified, and specific surface area increases, while adsorption capacity
Enhancing.Using loess particle as carrier, loading nanometer Fe nton photochemical catalysts should have both at low cost, environmental-friendly, absorption property
The features such as strong, to which there is good application prospect in photocatalytic degradation of dye waste water field.
Invention content
Purpose of the present invention is to the structure and characteristics using loess, provide a kind of loess loading nanometer Fe nton photochemical catalysts
Preparation method.
One, the preparation of loess loading nanometer Fe nton photochemical catalysts
The present invention is using loess as load agent, with FeSO4•7H2O is precursor, and water is dispersant, using in-situ reducing sedimentation
The obtained loess loading nanometer Fe nton photochemical catalysts of success.Concrete technology：By loess it is acidified after be scattered in distilled water be made
The loess suspension of a concentration of 20 ~ 200 g/L；Under inert gas protection, ferrous sulfate solution is added in loess suspension,
After the h of 0.5 h ~ 3.0 are stirred at room temperature, reducing agent is added and continues to be stirred to react the h of 1.0 h ~ 3.0；Deposition 10 is stood after reaction
The min of min ~ 60 after gained deposit is washed repeatedly with distilled water, are dried in vacuo the h of 3 h ~ 9 to get black at 60 DEG C ~ 90 DEG C
Powdered loess loading nanometer Fe nton photochemical catalysts.
The acidification of loess is scattered in loess in the HCl solution of 2 ~ 6 mol/L of concentration, the mechanical agitation at 65 ~ 85 DEG C
1.5 ~ 2.5 h, cooling, filtering, distillation are washed to neutrality, and 50 ~ 65 DEG C of 11 ~ 13 h of vacuum drying are to get acidification loess.
The addition of ferrous sulfate is be acidified loess quality 1.5 ~ 5.5 times.
Reducing agent is sodium borohydride or potassium borohydride, and the addition of reducing agent is 2 ~ 8 times of ferrous sulfate mole.
Two, the pattern of loess loading nanometer Fe nton photochemical catalysts and structural analysis
1, macro morphology
The macro morphology of loess loading nanometer Fe nton photochemical catalysts prepared by the present invention is as shown in Figure 1.It will be seen from figure 1 that
Loess loading nanometer Fe nton photochemical catalysts are black powder particle, and color is deeper, this is conducive to absorption of the catalyst to light.
In addition, black powder loess loading nanometer Fe nton photochemical catalysts have faint magnetism, recycling can be convenient for reuse.
2, infrared spectrum analysis
Fig. 2 is the infrared spectrum of loess loading nanometer Fe nton photochemical catalysts prepared by the present invention.In figure, 3600 ~ 3200 cm-1
Broad peak belongs to silicone hydroxyl（-OH）Stretching vibration absworption peak；1200~900 cm-1Absorption peak in range is attributed to silicate Si-
The asymmetric stretching vibration of O keys；780 cm-1Spike be Si-O in quartz stretching vibration peak, this illustrates depositing for loess particle
.Meanwhile 560 cm-1Spike belong to the vibration peaks of Fe-O keys, this is because the nano zero valence iron partial oxidation of load at
FeOOH.In short, IR shows Fenton photocatalysts in loess surface.
3, X-ray diffraction（XRD）Analysis
Phenetic analysis is carried out to loess loading nanometer Fe nton photochemical catalysts using XRD, the results are shown in Figure 3.In figure, acidification
The main component and characteristic peak of loess be respectively：Quartz（20.1°、26.6°、60°、67.5°）, chlorite（18.5°、25°）, she
Sharp stone（35°）And feldspar（28°）.Wherein, Quartz Characteristics peak is relatively strong.Ferro element information is as follows：Peak at 44.6 ° is nanometer
Zero-valent Iron（Fe0）Characteristic diffraction peak；Part is aoxidized Zero-valent Iron in the drying process, the Fe of generation2O3Diffraction maximum appear in
At 24.5 °, 35 °；The Fe of generation3O4The diffraction maximum that diffraction maximum is FeO present in 20 °, 30.1 °, at 21 °, wherein nanometer zero
The characteristic diffraction peak of valence iron is apparent, and the peak of other oxide components is weaker, illustrates compared to loess particle, iron oxide ratio compared with
It is low.
4, x-ray photoelectron spectroscopy（XPS）Analysis
Fig. 4 is the full spectrograms of XPS of loess loading nanometer Fe nton photochemical catalysts prepared by the present invention（a）With the fine spectrum of Fe2p
Figure.As can be seen that there are several essential elements of loess itself in composing entirely in XPS, i.e.,：Si2p（102.8）、O1s（532.1）、
C1s（284.8）And Ca（350.1）、Mg（311.5）、Ti（462.5）Deng.It is that the eV of 710 eV ~ 730 go out in electron binding energy
Very strong Fe2p characteristic peaks are showed.Further analyze the fine spectrogram of Fe2p, it can be seen that nanometer zero occur in 719.8eV
Valence iron（Fe0 2p1/2）Characteristic peak, illustrate that nano zero valence iron is successfully carried on loess surface, and ferrous iron occur（Fe2+）
And ferric iron（Fe3+）Peak, this is because catalyst exposure Fe in air0Caused by aoxidizing, also illustrate iron system Fenton
The presence of ingredient.
5, specific surface area and hole hold diameter analysis
Fig. 5 is loess loading nanometer Fe nton photochemical catalysts N prepared by the present invention2Adsorption-desorption isothermal（It is left）With aperture point
Butut（It is right）.It can be seen that its N2Adsorption-desorption isothermal curve belongs to the IV type thermoisopleths of mesoporous material, mesoporous material occurs
Expect typical H3 hysteresis loops.Its specific surface area is 28.8491 m2•g-1, pore volume 0.0720cm3•g-1, larger Kong Rongyu
Specific surface area is conducive to adsorb.
Three, the light degradation property of loess loading nanometer Fe nton photochemical catalysts
In order to investigate the catalytic degradation performance of loess loading nanometer Fe nton photochemical catalysts, with dyestuff（Basic fuchsin）It is dropped for target
Object is solved, is tested under visible light illumination, degradation property.Specific method：Take the Basic Fuchsin in Aqueous Solution of 50 mL（100 mg/L）In
In 100 mL conical flasks, pH to 2.36 is adjusted with concentrated hydrochloric acid, 0.05 g loess loading nanometer Fe nton photochemical catalysts are added（1 g/
L）、0.043 mL H2O2（8.5 mmol/L）, light source is opened, and carry out mechanical agitation, takes 5 mL to centrifuge at regular intervals, mistake
0.22 μm of filter membrane measures absorbance at 552 nm, calculates percent of decolourization.
The experimental results showed that loess loading nanometer Fe nton photochemical catalysts after 30 min of dark reaction to basic fuchsin
Percent of decolourization is 91.4%, and degradation rate can reach 100% after 30 min of illumination.Show loess loading nanometer Fe nton photochemical catalysts
There is excellent catalytic degradation performance to basic fuchsin under visible light illumination.
In conclusion the present invention is load agent with loess, with FeSO4•7H2O is precursor, and water is dispersant, using original position
Loess loading nanometer Fe nton photochemical catalysts have successfully been made in reduction sedimentation.The catalyst shows organic dyestuff excellent
Photocatalytic Degradation Property, and raw material is easy to get, it is of low cost.Under visible light illumination, which leads in dye wastewater treatment
Domain has good application prospect.
Description of the drawings
Fig. 1 is loess loading nanometer Fe nton photochemical catalyst macro morphology figures.
Fig. 2 is loess loading nanometer Fe nton photochemical catalyst infrared spectrograms.
Fig. 3 is loess loading nanometer Fe nton photochemical catalyst XRD diagram.
Fig. 4 is the fine spectrogram of the full spectrograms of XPS and Fe 2p of composite catalyst and its raw material loess.
Fig. 5 is loess loading nanometer Fe nton photochemical catalysts N2Adsorption-desorption isothermal and graph of pore diameter distribution.
Specific implementation mode
The preparation to loess loading nanometer Fe nton photochemical catalysts of the present invention and photocatalytic below by specific embodiment
It can be described further.
Embodiment 1
It weighs 1 g acidification loess and is scattered in 40 mL distilled water to obtain loess suspension；Weigh 0.99 g FeSO4•7H2O dissolves
It in 60 mL distilled water, is then added in loess suspension, leads to argon gas, be added 14.3 after 30 min of mechanical agitation at room temperature
The NaBH of mL4Solution（1 mol/L）, continue to be stirred to react 1 h, deposit, be washed with distilled water 4 ~ 5 times, 80 DEG C of vacuum drying 6
H obtains loess loading nanometer Fe nton photochemical catalysts.The photochemical catalyst is 95.3% to the removal rate of basic fuchsin.
Embodiment 2
It weighs 1.7 g acidification loess and is scattered in 45 mL distilled water to obtain loess suspension；Weigh 3.26 g FeSO4•7H2O is molten
Solution is then added in 60 mL distilled water in loess suspension, is led to nitrogen, is added after 30 min of mechanical agitation at room temperature
The KBH of 14.3 mL4Solution（1 mol/L）, continue to be stirred to react 1 h, deposit, be washed with distilled water 4 ~ 5 times, 80 °C of vacuum are dry
Dry 6 h obtains loess loading nanometer Fe nton photochemical catalysts.The photochemical catalyst is 96.8% to the removal rate of basic fuchsin.
Embodiment 3
It weighs 1.3 g acidification loess and is scattered in 40 mL distilled water to obtain loess suspension；Weigh 2.95 g FeSO4•7H2O is molten
Solution is then added in 60 mL distilled water in loess suspension, is led to argon gas, is added 35 after 30 min of mechanical agitation at room temperature
The NaBH of mL4Solution（1 mol/L）, continue to be stirred to react 1 h, deposit, be washed with distilled water 4 ~ 5 times, 80 DEG C of vacuum drying 6
H obtains loess loading nanometer Fe nton photochemical catalysts.The photochemical catalyst is 97.9% to the removal rate of basic fuchsin.
Embodiment 4
It weighs 2 g acidification loess and is scattered in 60 mL distilled water to obtain loess suspension；Weigh 5 g FeSO4•7H2O is dissolved in 80
It in mL distilled water, is then added in loess suspension, leads to nitrogen, be added 70 mL's after 30 min of mechanical agitation at room temperature
KBH4Solution（1 mol/L）, continue to be stirred to react 1 h, deposit, be washed with distilled water 4 ~ 5 times, 80 DEG C of 6 h of vacuum drying are obtained
Loess loading nanometer Fe nton photochemical catalysts.The photochemical catalyst is 99.8% to the removal rate of basic fuchsin.
In the various embodiments described above, the acidification of loess is distributed to loess in the HCl solution of 4 mol/L of concentration, at 80 DEG C
Lower mechanical agitation 2 hours, cooling, filtering, distillation are washed to neutrality, and 60 DEG C are dried in vacuo 12 hours to get acidification loess.
Claims (6)
1. a kind of preparation method of loess loading nanometer Fe nton photochemical catalysts, be by loess it is acidified after be scattered in distilled water
Loess suspension is made；Under inert gas protection, ferrous sulfate solution is added in loess suspension, be stirred at room temperature 0.5 h ~
After 3.0 h, reducing agent is added and continues to be stirred to react the h of 1.0 h ~ 3.0；The deposition min of 10 min ~ 60, institute are stood after reaction
Deposit is obtained to be washed with distilled water, it is dry to get black powder loess loading nanometer Fe nton photochemical catalysts.
2. a kind of preparation method of loess loading nanometer Fe nton photochemical catalysts as described in claim 1, it is characterised in that：Loess
Acidification be to be scattered in loess in the HCl solution of 2 ~ 6 mol/L of concentration, 1.5 ~ 2.5 h of mechanical agitation, cold at 65 ~ 85 DEG C
But, it filters, distillation is washed to neutrality, and 50 ~ 65 DEG C of 11 ~ 13 h of vacuum drying are to get acidification loess.
3. a kind of preparation method of loess loading nanometer Fe nton photochemical catalysts as described in claim 1, it is characterised in that：Sulfuric acid
Ferrous addition is be acidified loess quality 1.5 ~ 5.5 times.
4. a kind of preparation method of loess loading nanometer Fe nton photochemical catalysts as described in claim 1, it is characterised in that：Reduction
Agent is sodium borohydride or potassium borohydride, and the addition of reducing agent is 2 ~ 8 times of ferrous sulfate mole.
5. a kind of preparation method of loess loading nanometer Fe nton photochemical catalysts as described in claim 1, it is characterised in that：It is described
In loess suspension, the content of loess is 20 ~ 200g/L.
6. a kind of preparation method of loess loading nanometer Fe nton photochemical catalysts as described in claim 1, it is characterised in that：It is dry
It is that the h of 3 h ~ 9 are dried in vacuo at 60 DEG C ~ 90 DEG C.
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