CN106902731A - A kind of loess loaded titanium dioxide photocatalyst and preparation method thereof - Google Patents
A kind of loess loaded titanium dioxide photocatalyst and preparation method thereof Download PDFInfo
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- CN106902731A CN106902731A CN201710162905.2A CN201710162905A CN106902731A CN 106902731 A CN106902731 A CN 106902731A CN 201710162905 A CN201710162905 A CN 201710162905A CN 106902731 A CN106902731 A CN 106902731A
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- dioxide photocatalyst
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 58
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 9
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003112 inhibitor Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 239000002689 soil Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- 238000001354 calcination Methods 0.000 abstract description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- 239000010919 dye waste Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 13
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 13
- 229960000907 methylthioninium chloride Drugs 0.000 description 13
- 238000006731 degradation reaction Methods 0.000 description 11
- 230000015556 catabolic process Effects 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000000843 powder Substances 0.000 description 7
- 238000004042 decolorization Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 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 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 206010011376 Crepitations Diseases 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 241001251094 Formica Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011022 opal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
-
- B01J35/39—
-
- B01J35/50—
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F2101/308—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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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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)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
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Abstract
The invention discloses a kind of preparation method of loess loaded titanium dioxide photocatalyst, it is that ammonium chloride is nitrogen source, and acetic acid is inhibitor using loess as load agent, butyl titanate is presoma, and nitrogen doped titania original position is carried on into loess particle surface by sol-gal process；Then by calcining, loess loaded titanium dioxide photocatalyst is obtained.Photocatalytic degradation organic wastewater test result indicate that, loess loaded titanium dioxide photocatalyst prepared by the present invention has photocatalytic activity very high under simulated solar light irradiation, it is with low cost and raw material is easy to get, there is good application prospect in photocatalytic degradation of dye waste water field.
Description
Technical field
The present invention relates to a kind of titanium dioxide optical catalyst, more particularly to a kind of loess loaded titanium dioxide photocatalyst and
Its preparation method, belongs to composite science field and photocatalysis field.
Background technology
In recent years, problem of environmental pollution threatens the production and living of the mankind always, and water pollution problems is especially serious, industry print
Therefore the treatment for contaminating waste water gives more sustained attention and urgent problem as waste water industry.Photocatalysis technology is convenient fast due to it
Prompt, environmental protection, and extensive research has been obtained to the utilization of sunshine, especially nano titanium oxide, special semiconductor junction
Structure makes it have catalysis activity higher, and organic pollution that can be in different environments to difficult degradation plays efficient degradation effect,
And have the advantages that nontoxic, non-secondary pollution, stability are high.Certainly, pure nano titanium oxide also has some defects, such as：Prohibit
Band is wider, quantum efficiency is low；The shortcomings of particle is too thin, easily reunion, hardly possible are reclaimed.Research shows：Doping vario-property（Such as：Metal ion
Doping, nonmetallic ion-doped, ion co-doped etc.）Its energy gap can be made to narrow such that it is able to absorbing wavelength it is longer can
See light, improve the utilization rate to sunshine.In order to improve some shortcomings that nano titanium oxide exists in actual applications（Such as：
Particle is too thin, easily reunites in actual application, reclaims difficult in water solution system, is not easy to aqueous phase separation etc.）, can be by dioxy
Change titanium and load to inorganic, organic polymer carrier.
Clay effective carrier as first stability, for load nano-titanium dioxide, such as：Sun etc.（Applied
Catalysis A: General, 2013, 458: 103-110.）Using hydrolysis deposition be prepared for three kinds it is porous amorphous
Silica（Diatomite, opal, porous precipitated silica）Loaded titanium dioxide photocatalyst, finds silica supports
Property can influence the crystalline structure of particle size and titanium dioxide, under ultraviolet light during rhodamine B degradation, diatomite is born
Carrying of titanium dioxide reaches 85% to the percent of decolourization of rhodamine B.Lv Jun etc.（Material heat treatment journal, 2010, (12):19-23）Using
Hydrolysis methods are prepared for mica load nano-titanium dioxide catalyst, it is found that it has light degradation property to methyl orange.Cui Hao etc.
（CN104888777A）It is prepared for a kind of attapulgite clay-TiO2-Cu2The compound visible light catalysts of O, composite catalyst exists
Visible region has response, and catalytic degradation efficiency is high, it is possible to use Visible Light Induced Photocatalytic organic matter.Su Lei etc.（CN105797762A）Adopt
Haydite is made with the raw material such as sludge, clay, activated carbon or wood chip, calcium hydroxide, the Sm doping two being made up of sol-gal process
Nano titanium oxide powder, by hydro-thermal method, the technique such as vapor-phase sintering obtains a kind of photocatalysis haydite under condition of nitrogen gas.Guo Yingqing etc.
（CN201610477453.2）Disclose the preparation method that a kind of near infrared light is catalyzed column clay catalyst.These methods respectively have
Characteristic.However, in order to be more beneficial for the popularization and application of such catalyst, it is necessary to find more cheap and effective carrier material.
Loess is a kind of wide material sources, natural inorganic material cheap and easy to get, and its loose lamellar structure makes it have necessarily
Adsorption capacity, it is acidified it is modified after, specific surface area increase, while adsorption capacity strengthens.Therefore, nonmetallic nitrogen will be doped with
Titanium dichloride load to acidified treated loess particle surface, both performances is acted synergistically, can turn into excellent
Catalysis material be applied in wastewater treatment.
The content of the invention
The present invention seeks to junction structure and characteristic using loess, there is provided a kind of loess loaded titanium dioxide photocatalyst
Preparation method.
First, the preparation of loess loaded titanium dioxide photocatalyst
The preparation method of loess loaded titanium dioxide photocatalyst of the present invention, is by sol-gal process that nitrogen doped titania is former
Position is carried on loess particle surface.Concrete technology is：Acidifying loess is scattered in alcohol-water mixed solution, adds ammonium chloride to make
It is nitrogen source, acetic acid obtains loess mixed liquor as inhibitor, and with concentrated acid regulation system pH=1 ~ 3；It is again that butyl titanate is equal
It is even to be scattered in the solution of tetrabutyl titanate that absolute ethyl alcohol is obtained, it is added in above-mentioned loess mixed liquor, stir 20 ~ 30 minutes and formed
Colloidal sol；40 ~ 75 DEG C are then heated to, gel is formed within still aging 6 ~ 36 hours, dried, pulverized；Finally at 350 ~ 650 DEG C
Calcining 0.5 ~ 3 hour, obtains loess loaded titanium dioxide photocatalyst.
The preparation of the acidifying loess, is that loess is distributed in the HCl solution of the mol/L of concentration 1 ~ 5, at 45 ~ 85 DEG C
Mechanical agitation 1 ~ 5 hour, cooling, filtering, distillation is washed to neutrality, and 40 ~ 80 DEG C are vacuum dried 6 ~ 36 hours, obtain final product acidifying yellow
Soil.
In the alcohol-water mixed solution, alcohol is the ethanol of absolute ethyl alcohol, methyl alcohol or mass fraction 75% ~ 95%；Water and alcohol
Volume ratio is 1:1 ~1:6；In loess mixed liquor, the dispersion amount for being acidified loess is 0.05 ~ 0.02g/mL.
Nitrogen source ammonium chloride addition is be acidified loess quality 0.01 ~ 0.03 times.
Inhibitor acetic acid addition is that 1 ~ 5 mL/g is acidified loess.
Butyl titanate is 1 ~ 5 mL/g with the mass volume ratio of acidifying loess.
In the solution of tetrabutyl titanate, butyl titanate and absolute ethyl alcohol volume ratio are 1:1~1:5.
The concentrated acid is the concentrated nitric acid of concentration 60% ~ 68%.
2nd, loess loaded titanium dioxide photocatalyst pattern and structural analysis
1st, macroscopic view and microscopic appearance
Fig. 1 is the macro morphology figure of loess loaded titanium dioxide photocatalyst prepared by the present invention.It will be seen from figure 1 that loess
Loaded titanium dioxide photocatalyst is gray powdery particle, darker compared with loess is acidified, and this is also beneficial to catalysis
Absorption of the agent to light.
The microscopic appearance of loess loaded titanium dioxide photocatalyst using scanning electron microscopic observation, is as a result shown in Fig. 2, wherein a
It is natural loess, b is acidifying loess, and c is the loess of carried titanium dioxide.From scanning electron microscope (SEM) photograph as can be seen that loess load two
Titania photocatalyst surface porosity, there is more crackles, and the nano level titanium dioxide granule of area load, and this also says
The degraded of loess loaded titanium dioxide photocatalyst prepared by the bright present invention to pollutant is suction-operated and the titanium dioxide of loess
The result of the light degradation synergy of titanium.
2nd, infrared spectrum analysis
Fig. 3 is the infrared spectrum of loess loaded titanium dioxide photocatalyst, wherein 470cm-1Place is the stretching vibration of Ti-O keys,
1026cm-1It is nearby the stretching vibration absworption peak of Si-O-Si, 3000 ~ 3500cm-1The absworption peak wide for nearby occurring is titanium dioxide
What the O-H stretching vibrations on titanium surface caused, 720cm-1It is nearby the characteristic absorption peak of quartz, compared to loess particle, loess is born
This peak is weaker in carrying of titanium dioxide photocatalyst, and this is probably the reason due to calcining.From the figure 3, it may be seen that the structure of loess particle
It is basic to keep, it is also possible to detect the characteristic peak of titanium dioxide, illustrate that composite is made up of loess and titanium dioxide, this also with
SEM results are consistent.
3rd, XRD analysis
Fig. 4 is the XRD of loess carried titanium dioxide, wherein the diffraction maximum in 25.38 °, 37.73 °, 48.11 ° appearance is right respectively
Answer sharp titanium phase titanic oxide（101）、（004）、（200）Crystal face, the very strong of appearance is spread out at 20.86 °, 48.11 ° and 50.13 °
The characteristic diffraction peak that peak is quartz in loess is penetrated, 28 ° of diffraction maximums for nearby occurring are amorphous silicate or aluminosilicate in loess
The characteristic diffraction peak of salt, these all illustrate that composite is made up of loess and titanium dioxide, and titanium dioxide is in mainly sharp titanium
Phase crystal formation, and the addition of loess does not have an impact the crystal formation of titanium dioxide.
3rd, the light degradation property test of loess loaded titanium dioxide photocatalyst
Methylene blue is lived as a kind of representational pollutant, the photocatalysis for testing loess load nitrogen-doped titanium dioxide
Property.The photochemical catalyst of 0.05g is weighed, the methylene blue solution of 50mL is distributed to（C=20mg/L）In, dark reaction 20min reaches suction
Attached desorption equilibrium, then the magnetic agitation 135min under 800w xenon sources, takes the centrifugation of 5mL samples, upper liquid at regular intervals
By 0.22 μm of filter membrane, the concentration of remaining methylene blue is determined using ultraviolet-visible spectrophotometry, calculate percent of decolourization.
Fig. 5 is the light degradation curve map to methylene blue under different catalysts and different condition.From fig. 5, it can be seen that yellow
Native carried titanium dioxide reaches 57.3% after dark reaction 20min to the clearance of methylene blue, and clearance reaches after illumination 135min
To 94.2%, and under non-illuminated conditions, it is held essentially constant after clearance reaches 60% after 135min, illustrates loess load two
Titanium oxide has certain adsorption capacity to methylene blue, and mainly photocatalytic degradation plays Main Function after opening light source.And
Nitrogen-doped titanium dioxide after dark reaction 20min to methylene blue substantially without removal, clearance persistently rises after illumination.Tie above
Fruit explanation loess carried titanium dioxide composite photo-catalyst has good catalytic degradation under simulated solar irradiation to methylene blue
Performance, and degradation reaction is absorption and the result of nitrogen-doped titanium dioxide synergy of loess particle.
In sum, using loess as load agent, ammonium chloride is nitrogen source to the present invention, and acetic acid is inhibitor, butyl titanate
It is presoma, nitrogen doped titania original position is carried on by loess particle surface by sol-gal process；Then by calcining, it is obtained
Loess loaded titanium dioxide photocatalyst.Photocatalytic degradation organic wastewater result shows that the loess prepared by the present invention loads two
Titania photocatalyst has photocatalytic activity very high under simulated solar light irradiation, and raw material is easy to get, with low cost.Therefore
There is good application prospect in photocatalytic degradation of dye waste water field.
Brief description of the drawings
Fig. 1 is the macro morphology figure of loess carried titanium dioxide.
Fig. 2 is loess carried titanium dioxide and its raw material（Loess, acidifying loess）Scanning electron microscope (SEM) photograph.In figure：（a）It is Huang
Soil；（b）It is acidifying loess；（c）It is loess carried titanium dioxide.
Fig. 3 is the infrared absorpting light spectra of loess carried titanium dioxide.
Fig. 4 is the XRD of loess carried titanium dioxide.
Fig. 5 is the light degradation curve map to methylene blue under different catalysts and different condition.
Specific embodiment
The preparation to loess loaded titanium dioxide photocatalyst of the present invention and photocatalysis performance below by specific embodiment
It is described further.
Embodiment 1
0.5 g acidifying loess is taken, 10 mL alcohol-water mixed solutions are scattered in（Water and ethanol volume ratio are 1:1）In, add
0.01g ammonium chlorides, 0.1mL acetic acid, and use concentrated nitric acid（67%）Regulation system pH=2, obtains loess mixed liquor.
Take 1mL butyl titanates to be scattered in 5 mL ethanol, stir, obtain solution of tetrabutyl titanate.By metatitanic acid four
Butyl acetate solution is added in loess mixed liquor, is stirred 20 ~ 30 minutes, and 75 DEG C, still aging 6 ~ 36 hours are warming up to after forming colloidal sol
Formed gel, 80 DEG C vacuum drying 30 hours after pulverize.650 DEG C are placed in Muffle furnace again to calcine 0.5 hour, obtain Huang
Native loaded titanium dioxide photocatalyst.
The photochemical catalyst is 77.3% to the percent of decolourization of methylene blue.
Embodiment 2
1.0g acidifying loess is taken, 50mL alcohol-water mixed solutions are scattered in（Water and ethanol volume ratio are 1:6）In, add 0.1g
Ammonium chloride, 0.5 mL acetic acid, and use concentrated nitric acid（67%）Regulation system pH=2, obtains loess mixed liquor.
Take and 3mL butyl titanates are scattered in 10 mL ethanol, stir, obtain solution of tetrabutyl titanate.By metatitanic acid
Four butyl acetate solutions are added in loess mixed liquor, are stirred 20 ~ 30 minutes, and 40 DEG C are warming up to after forming colloidal sol, and still aging 30 ~ 36 is small
When form gel, 65 DEG C are vacuum dried 48 hours, grind to form powder.Powder is placed in Muffle furnace again, 400 DEG C of calcinings 2.5 are small
When, obtain loess loaded titanium dioxide photocatalyst.
The photochemical catalyst is 94.0% to the percent of decolourization of methylene blue.
Embodiment 3
1.5 g acidifying loess is taken, 120mL alcohol-water mixed solutions are scattered in（Water and ethanol volume ratio are 1:3）In, add
0.3g ammonium chlorides, 3mL acetic acid, and use concentrated nitric acid（67%）Regulation system pH=2, obtains loess mixed liquor；
6mL butyl titanates are scattered in 30 mL ethanol, are stirred, obtain solution of tetrabutyl titanate.By butyl titanate
Solution is added in above-mentioned loess mixed liquor, is stirred 20 ~ 30 minutes, and 55 DEG C, still aging 6 ~ 36 hours are warming up to after forming colloidal sol
Gel is formed, 55 DEG C are vacuum dried 48 hours, grind to form powder.Powder is placed in Muffle furnace into 550 DEG C again to calcine 1.5 hours,
Obtain loess loaded titanium dioxide photocatalyst.
The photochemical catalyst is 98.0% to the percent of decolourization of methylene blue.
Embodiment 4
Take 2.5 g acidifying loess and be scattered in 150mL alcohol-water mixed solutions（Water and ethanol volume ratio are 1:5）In, add 0.5g
Ammonium chloride, 5 mL acetic acid, and use concentrated nitric acid（67%）Regulation system pH=2, obtains loess mixed liquor.
10 mL butyl titanates are scattered in 50 mL ethanol, are stirred, obtain solution of tetrabutyl titanate.By metatitanic acid
Four butyl acetate solutions are added in above-mentioned loess mixed liquor, are stirred 20 ~ 30 minutes, and 55 DEG C, still aging 36 are warming up to after forming colloidal sol
Hour forms gel, and 30 DEG C are vacuum dried 48 hours, grind to form powder.Powder is placed in 350 DEG C of calcinings 3 in Muffle furnace again small
When, obtain loess loaded titanium dioxide photocatalyst.
The photochemical catalyst is 98.5% to the percent of decolourization of methylene blue.
Claims (9)
1. a kind of preparation method of loess loaded titanium dioxide photocatalyst, is that acidifying loess is scattered in into alcohol-water mixed solution
In, add ammonium chloride as nitrogen source, acetic acid obtains loess mixed liquor as inhibitor, and with concentrated acid regulation system pH=1 ~ 3；Again
Butyl titanate is dispersed in the solution of tetrabutyl titanate that absolute ethyl alcohol is obtained, is added in above-mentioned loess mixed liquor, stirred
Mix 20 ~ 30 minutes and form colloidal sol；40 ~ 75 DEG C are then heated to, gel is formed within still aging 6 ~ 36 hours, dried, pulverized；
It is last to be calcined 0.5 ~ 3 hour at 350 ~ 650 DEG C, obtain loess loaded titanium dioxide photocatalyst.
2. as claimed in claim 1 a kind of preparation method of loess loaded titanium dioxide photocatalyst, it is characterised in that：Acidifying is yellow
The preparation of soil, is that loess is distributed in the HCl solution of the mol/L of concentration 1 ~ 5, and mechanical agitation 1 ~ 5 hour, cold at 45 ~ 85 DEG C
But, filter, distillation is washed to neutrality, 40 ~ 80 DEG C are vacuum dried 6 ~ 36 hours, obtain final product acidifying loess.
3. as claimed in claim 1 a kind of preparation method of loess loaded titanium dioxide photocatalyst, it is characterised in that：Loess is mixed
Close in liquid, the dispersion amount for being acidified loess is 0.05 ~ 0.02g/mL.
4. as claimed in claim 1 a kind of preparation method of loess loaded titanium dioxide photocatalyst, it is characterised in that：It is described
In alcohol-water mixed solution, alcohol is the ethanol of absolute ethyl alcohol, methyl alcohol or mass fraction 75% ~ 95%；The volume ratio of water and alcohol is 1:1~
1:6。
5. as claimed in claim 1 a kind of preparation method of loess loaded titanium dioxide photocatalyst, it is characterised in that：Nitrogen source chlorine
It is be acidified loess quality 0.01 ~ 0.03 times to change ammonium addition.
6. as claimed in claim 1 a kind of preparation method of loess loaded titanium dioxide photocatalyst, it is characterised in that：Inhibitor
Acetic acid addition is that 1 ~ 5 mL/g is acidified loess.
7. as claimed in claim 1 a kind of preparation method of loess loaded titanium dioxide photocatalyst, it is characterised in that：Metatitanic acid four
Butyl ester is 1 ~ 5 mL/g with the mass volume ratio of acidifying loess.
8. as claimed in claim 1 a kind of preparation method of loess loaded titanium dioxide photocatalyst, it is characterised in that：The titanium
In sour four butyl acetate solutions, butyl titanate and absolute ethyl alcohol volume ratio are 1:1~1:5.
9. as claimed in claim 1 a kind of preparation method of loess loaded titanium dioxide photocatalyst, it is characterised in that：It is described dense
Acid is the concentrated nitric acid of concentration 60% ~ 68%.
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