CN108355633A - A kind of preparation method of visible light-responded nitrating nanometer titanium dioxide photochemical catalyst - Google Patents
A kind of preparation method of visible light-responded nitrating nanometer titanium dioxide photochemical catalyst Download PDFInfo
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- CN108355633A CN108355633A CN201810107004.8A CN201810107004A CN108355633A CN 108355633 A CN108355633 A CN 108355633A CN 201810107004 A CN201810107004 A CN 201810107004A CN 108355633 A CN108355633 A CN 108355633A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 28
- 239000003054 catalyst Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 230000000802 nitrating effect Effects 0.000 title claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 29
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 24
- 239000000919 ceramic Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000011261 inert gas Substances 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 12
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 12
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 239000010936 titanium Substances 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- XFVGXQSSXWIWIO-UHFFFAOYSA-N chloro hypochlorite;titanium Chemical compound [Ti].ClOCl XFVGXQSSXWIWIO-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000003086 colorant Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000001782 photodegradation Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 150000003609 titanium compounds Chemical class 0.000 claims description 2
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract 1
- 235000010215 titanium dioxide Nutrition 0.000 description 30
- 239000000047 product Substances 0.000 description 25
- 230000007547 defect Effects 0.000 description 10
- 230000003287 optical effect Effects 0.000 description 7
- 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 7
- 229940043267 rhodamine b Drugs 0.000 description 7
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910003081 TiO2−x Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical group [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003608 titanium Chemical class 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
- 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
-
- 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
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
-
- 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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- 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
The present invention provides a kind of preparation methods of visible light-responded nitrating nanometer titanium dioxide photochemical catalyst, and ascorbic acid and urea are added in deionized water, clear solution is stirred to get；Trivalent titanium solution and sodium hydroxide solution are added, it is 1.5 ~ 5 to adjust pH value, persistently stirs to get brown or blood-red solution；Solution is transferred in water heating kettle, brown color head product is obtained by the reaction at 180 DEG C of temperature；It is 7 that brown color head product, which is passed through washing to pH, is dried overnight, obtains black product, is brown ceramic powder after grinding；Brown ceramic powder is placed in the tube furnace under inert gas shielding, and is that 0.03 ~ 0.08atm is down to room temperature in 400 ~ 500 DEG C of temperature calcining at constant temperature 2 ~ 4 hours by controlling vacuum pump to adjust vacuum degree, obtains visible light-responded nitrogen-doped nanometer titanium dioxide material.Invention enhances photochemical catalysts in ultraviolet, visible and near-infrared light absorpting ability.
Description
Technical field
The invention belongs to materialogy fields, are related to a kind of photocatalysis material of titanium dioxide, specifically a kind of visible light
Respond the preparation method of nitrating nanometer titanium dioxide photochemical catalyst.
Background technology
Nano-titanium dioxide（TiO2）Photochemical catalyst has many advantages, such as that nontoxic, inexpensive and chemical stability is high, the catalysis
Agent can the efficiently and safely organic pollutions such as decomposing formaldehyde, rhodamine B and hydrogen production by water decomposition under the excitation of light.But
Untreated white titania lower quantum efficiency and the problems such as compound higher photo-generated carrier under full spectrum,
Seriously limit its practical application in photocatalysis field.
In recent years, domestic and international researcher constructed by metal/non-metal doping, hetero-junctions, the means such as photosensitizer sensitization
Successfully improve the full spectral absorption performance of titanic oxide material.In addition, passing through itself Ti3+Or oxygen defect（Vo）Introducing prepare
The reduction titanium dioxide of different colours（TiO2-x）Also can be promoted material photo-catalysis capability (Science 2011,331,
746).Studies have shown that Ti3+The distribution of/Vo defects and concentration are to modified TiO2-xLight absorption and carrier separation efficiency tool
It has a major impact, these defects can be in TiO2 Localized modes are introduced in forbidden band and then reduce band gap width, improve the visible light of material
Absorbability.But the Ti excessively introduced3+/ Vo defects can form the new complex centre of photo-generated carrier, and defect concentrates on sample
The TiO on product surface2-xMaterial also deposits the shortcomings of stability is poor in air.On the other hand, due to nitrogen oxygen atom radius phase
Closely, nitrogen is easier to the structure that doping introduces titanium dioxide.N doping can improve TiO by reducing photochemical catalyst energy gap2Light is urged
Change the light absorpting ability of material, while Ti can be stablized3+/ Vo defects improve reduction titanium dioxide stability (Energy
Environ. Sci. 2014,7,967).In conclusion binding deficient auto-dope and the preparation of N doping technique are stable and efficient
Reduction TiO2Play an important roll for improving photocatalyst activity.
Invention content
For above-mentioned technical problem in the prior art, the present invention provides a kind of visible light-responded nitrating nanometer titanium dioxides
The preparation method of the preparation method of titanium photochemical catalyst, this visible light-responded nitrating nanometer titanium dioxide photochemical catalyst is wanted
The technical problem that the visible light catalysis activity that solves photocatalysis material of titanium dioxide in the prior art is not high, stability is not high.
The present invention provides a kind of preparation method of visible light-responded nitrating nanometer titanium dioxide photochemical catalyst, including it is as follows
Step：
1) ascorbic acid and urea are added in deionized water, the material ratio of the ascorbic acid, urea and deionized water is
0.5~1g：5~50mg：35 ~ 50mL stirs to get clear solution；
2) to step 1）Solution in be added trivalent titanium solution, the mass volume ratio of the titanous and above-mentioned clear solution is
2~10g:20 ~ 100ml, the trivalent titanium compound are titanium trichloride and titanium oxychloride, add sodium hydroxide solution, described
Sodium hydroxide solution 0.2 ~ 1.5mo/L of concentration, adjust pH value be 1.5 ~ 5, under 250 ~ 1000r/min speed conditions continue
Stirring 0.5 ~ 2 hour, obtains brown or blood-red solution；
3) by step 2）Solution be transferred in water heating kettle, reacted 8 ~ 12 hours at 180 DEG C of temperature, obtain brown color primiparity
Object；
4) by step 3）Brown color head product to be washed to pH by deionized water and ethyl alcohol be 7, be dried overnight, obtain black production
Object is carefully brown ceramic powder after grinding；
5) by step 4）Brown ceramic powder be placed in the tube furnace under inert gas shielding, and pass through control vacuum pump adjust vacuum
Degree is that -0.03 ~ -0.08atm is down to room temperature in 400 ~ 500 DEG C of temperature calcining at constant temperature 2 ~ 4 hours, obtains visible light-responded nitrogen and mixes
Miscellaneous nanometer titanic oxide material.
Further, by step 4）Middle brown ceramic powder is placed in inert gas（Nitrogen or argon gas）In tube furnace under protection,
And when by controlling vacuum pump to adjust vacuum degree being -0.03 ~ -0.08atm, in 400 ~ 500 DEG C of temperature calcining at constant temperature 2 hours, drop
To room temperature, grey powder is obtained.
Further, by step 4）Middle brown ceramic powder is placed in inert gas（Nitrogen or argon gas）In tube furnace under protection,
And when by controlling vacuum pump to adjust vacuum degree being -0.03 ~ -0.08atm, in 400 ~ 500 DEG C of temperature calcining at constant temperature 2 hours, drop
To room temperature, buff powder is obtained.
Further, step 1）Mixing speed be 250 ~ 1000r/min.
Further, the inert gas is nitrogen or argon gas.
The present invention also provides a kind of purposes of above-mentioned visible light-responded nitrogen-doped nanometer titanium dioxide catalyst, the materials
Water is catalytically decomposed for the purification at air and water source, automatically cleaning, sun photodegradation water or solar photoelectric in material.
The present invention is using trivalent titanium salt as raw material, and ascorbic acid is reducing agent, and urea is nitrogen source, in conjunction with hydro-thermal method and high temperature
Calcination process prepares nitrating nanometer titanium dioxide photochemical catalyst.By introducing oxygen defect and nitrogen member in titanium dioxide optical catalyst
Element adjusts titanic oxide material in ultraviolet, visible and near infrared region absorbing properties, enhances titanic oxide material complete
The light absorpting ability of spectrum.Meanwhile speed and high-temperature roasting vacuum degree is mixed by controlling presoma, control product property
And color, the crystallinity and defect density of nano-titanium dioxide are adjusted, and then improve its photocatalytic activity.It is according to the present invention
Preparation process is mild, than traditional hydrogen or sodium borohydride nano-TiO2Method of modifying is safer, can also be by roasting
The different adjustment product characteristics of vacuum degree in journey.
The present invention is compared with prior art, and technological progress is significant.The present invention passes through in titanium dioxide optical catalyst
Middle introducing oxygen defect and nitrogen enhance photochemical catalyst in ultraviolet, visible and near-infrared light absorpting ability.Knot of the present invention
It closes hydro-thermal method and high-temperature roasting processing can meet different compared with the color, crystallinity and defect density of accuracy controlling titanium dioxide
Use environment.
Description of the drawings
Fig. 1 be black of the present invention, grey, light yellow nano titanium dioxide photocatalyst photo figure, wherein a is black sample
Product, b are grey sample, and c is light yellow sample.
Fig. 2 is the UV, visible light solid diffusing reflection abosrption spectrogram of light yellow titania powder prepared by embodiment 1.
Fig. 3 is the XRD spectrum of light yellow titania powder prepared by embodiment 1.
Fig. 4 is the scanning electron microscope collection of illustrative plates and elemental analysis figure of light yellow titania powder prepared by embodiment 1.
Fig. 5 is the transmission electron microscope collection of illustrative plates of light yellow titania powder prepared by embodiment 1.
Fig. 6 is light yellow titanium dioxide and P25 type black titanium dioxides degradation RhB effects prepared by embodiment 1 and embodiment 2
Fruit comparison diagram.
Specific implementation mode
Below by embodiment to carry out basic description to the present invention, it is necessary to which indicated herein is that the present embodiment is only used
In invention is further explained, it should not be understood as the limitation to invention protection domain, the person skilled in the art in the field
Some the nonessential modifications and adaptations that can be made according to the content of aforementioned present invention.
Embodiment 1
A, 0.5g ascorbic acid and 40mg urea are added in 35mL deionized waters, obtain clear solution；
B, 1.5mL trivalent titanium solutions are added into step a solution, add the sodium hydroxide solution of 1mol/L, adjusting pH value is
4, it is persistently stirred under 500r/min speed conditions, obtains blood-red solution；
C, solution in step b is transferred in water heating kettle, is reacted 8 hours at 180 DEG C of temperature, obtains brown color head product；
D, it is 7 brown color head product in step c to be washed 3 ~ 5 times to pH by deionized water and ethyl alcohol, is dried overnight, obtains black
Color product is carefully brown ceramic powder after grinding；
E, brown ceramic powder in step d is placed in the tube furnace under inert gas shielding, and vacuum is adjusted by controlling vacuum pump
When degree is -0.08atm, in 450 DEG C of temperature calcining at constant temperature 4 hours, it is down to room temperature, obtains light yellow titanium dioxide optical catalyst.
Embodiment 2
A, 0.5g ascorbic acid and 150mg urea are added in 35mL deionized waters, obtain clear solution；
B, 1.5mL trivalent titanium solutions are added into step a solution, add the sodium hydroxide solution of 1mol/L, adjusting pH value is
4, it is persistently stirred under 500r/min speed conditions, obtains blood-red solution；
C, solution in step b is transferred in water heating kettle, is reacted 8 hours at 180 DEG C of temperature, obtains brown color head product；
D, it is 7 brown color head product in step c to be washed 3 ~ 5 times to pH by deionized water and ethyl alcohol, is dried overnight, obtains black
Color product is carefully brown ceramic powder after grinding；
E, brown ceramic powder in step d is placed in the tube furnace under inert gas shielding, and vacuum is adjusted by controlling vacuum pump
When degree is -0.08atm, in 450 DEG C of temperature calcining at constant temperature 4 hours, it is down to room temperature, obtains light yellow titanium dioxide optical catalyst.
Embodiment 3
A, 0.5g ascorbic acid and 120mg urea are added in 35mL deionized waters, obtain clear solution；
B, 1.5mL trivalent titanium solutions are added into step a solution, add the sodium hydroxide solution of 1mol/L, adjusting pH value is
4, it is persistently stirred under 750r/min speed conditions, obtains blood-red solution；
C, solution in step b is transferred in water heating kettle, is reacted 8 hours at 180 DEG C of temperature, obtains brown color head product；
D, it is 7 brown color head product in step c to be washed 3 ~ 5 times to pH by deionized water and ethyl alcohol, is dried overnight, obtains palm fibre
Yellow product is carefully brown ceramic powder after grinding；
E, brown ceramic powder in step d is placed in the tube furnace under inert gas shielding, and vacuum is adjusted by controlling vacuum pump
When degree is -0.07atm, in 450 DEG C of temperature calcining at constant temperature 4 hours, it is down to room temperature, obtains light yellow titanium dioxide optical catalyst.
Embodiment 4
A, 0.5g ascorbic acid and 20mg urea are added in 35mL deionized waters, obtain clear solution；
B, 1.5mL trivalent titanium solutions are added into step a solution, add the sodium hydroxide solution of 1mol/L, adjusting pH value is
4, it is persistently stirred under 250r/min speed conditions, obtains brown solution；
C, solution in step b is transferred in water heating kettle, is reacted 12 hours at 180 DEG C of temperature, obtains brown color head product；
D, it is 7 brown color head product in step c to be washed 3 ~ 5 times to pH by deionized water and ethyl alcohol, is dried overnight, obtains palm fibre
Yellow product is carefully brown ceramic powder after grinding；
E, brown ceramic powder in step d is placed in the tube furnace under inert gas shielding, and vacuum is adjusted by controlling vacuum pump
When degree is -0.07atm, in 450 DEG C of temperature calcining at constant temperature 4 hours, it is down to room temperature, obtains light yellow titanium dioxide optical catalyst.
Embodiment 5
A, 0.5g ascorbic acid and 120mg urea are added in 35mL deionized waters, obtain clear solution；
B, 1.5mL trivalent titanium solutions are added into step a solution, add the sodium hydroxide solution of 1mol/L, adjusting pH value is
4, it is persistently stirred under 500r/min speed conditions, obtains blood-red solution；
C, solution in step b is transferred in water heating kettle, is reacted 8 hours at 180 DEG C of temperature, obtains brown color head product；
D, it is 7 brown color head product in step c to be washed 3 ~ 5 times to pH by deionized water and ethyl alcohol, is dried overnight, obtains black
Color product is carefully brown ceramic powder after grinding；
E, brown ceramic powder in step d is placed in the tube furnace under inert gas shielding, and vacuum is adjusted by controlling vacuum pump
When degree is -0.03atm, in 450 DEG C of temperature calcining at constant temperature 4 hours, it is down to room temperature, obtains grey titanium dioxide optical catalyst.
Embodiment 6
A, 0.5g ascorbic acid and 20mg urea are added in deionized water, obtain clear solution；
B, 1.5mL trivalent titanium solutions are added into step a solution, add the sodium hydroxide solution of 1mol/L, adjusting pH value is
4, it is persistently stirred under 750r/min speed conditions, obtains blood-red solution；
C, solution in step b is transferred in water heating kettle, is reacted 12 hours at 180 DEG C of temperature, obtains brown color head product；
D, it is 7 brown color head product in step c to be washed 3 ~ 5 times to pH by deionized water and ethyl alcohol, is dried overnight, obtains black
Color product is carefully brown ceramic powder after grinding；
E, brown ceramic powder in step d is placed in the tube furnace under inert gas shielding, and normal pressure is adjusted by controlling vacuum pump
When state, in 450 DEG C of temperature calcining at constant temperature 4 hours, it is down to room temperature, obtains black titanium dioxide photochemical catalyst.
The catalytic performance of grey titania powder prepared by 1 present invention of application example
The sample 1 and 20ppm rhodamine B solution 100mL for taking 10mg embodiments 1, are placed in beaker, are wrapped up with masking foil, is protected from light
It is stirred overnight, the solution being stirred is transferred in reaction vessel, open and visible filter is housed（λ>420nm）Mercury lamp light
Source carries out illumination to reaction solution, takes about 1.5mL solution at regular intervals, is placed in centrifuge tube, is centrifuged for 9000rpm in rotating speed
3min takes supernatant liquor, and the content of rhodamine B in supernatant is detected with ultraviolet-visible spectrophotometer.Obtain Fig. 6 test specimens
Product 1 are to rhodamine B degradation curve.
The catalytic performance of grey titania powder prepared by 2 present invention of application example
The sample 2 and 20ppm rhodamine B solution 100mL for taking 10mg embodiments 2, are placed in beaker, are wrapped up with masking foil, is protected from light
It is stirred overnight, the solution being stirred is transferred in reaction vessel, open and visible filter is housed（λ>420nm）Mercury lamp light
Source carries out illumination to reaction solution, takes about 1.5mL solution at regular intervals, is placed in centrifuge tube, is centrifuged for 9000rpm in rotating speed
3min takes supernatant liquor, and the content of rhodamine B in supernatant is detected with ultraviolet-visible spectrophotometer.Obtain Fig. 6 test specimens
Product 2 are to rhodamine B degradation curve.
Claims (4)
1. a kind of preparation method of visible light-responded nitrating nanometer titanium dioxide photochemical catalyst, it is characterised in that including walking as follows
Suddenly：
1）Ascorbic acid and urea are added in deionized water, the material ratio of the ascorbic acid, urea and deionized water is
0.5~1g：5~50mg：35 ~ 50mL stirs to get clear solution；
2）To step 1）Solution in be added trivalent titanium solution, the mass volume ratio of the titanous and above-mentioned clear solution is
2~10g:20 ~ 100ml, the trivalent titanium compound are titanium trichloride and titanium oxychloride, add sodium hydroxide solution, described
Sodium hydroxide solution 0.2 ~ 1.5mo/L of concentration, adjust pH value be 1.5 ~ 5, under 250 ~ 1000r/min speed conditions continue
Stirring 0.5 ~ 2 hour, obtains brown or blood-red solution；
3）By step 2）Solution be transferred in water heating kettle, reacted 8 ~ 12 hours at 180 DEG C of temperature, obtain brown color primiparity
Object；
4）By step 3）Brown color head product to be washed to pH by deionized water and ethyl alcohol be 7, be dried overnight, obtain black production
Object is carefully brown ceramic powder after grinding；
5）By step 4）Brown ceramic powder be placed in the tube furnace under inert gas shielding, and pass through control vacuum pump adjust vacuum
Degree is that -0.03 ~ -0.08atm is down to room temperature in 400 ~ 500 DEG C of temperature calcining at constant temperature 2 ~ 4 hours, obtains visible light-responded nitrogen and mixes
Miscellaneous nanometer titanic oxide material.
2. a kind of preparation method of visible light-responded nitrating nanometer titanium dioxide photochemical catalyst according to claim 1,
It is characterized in that：Step 1）Mixing speed be 250 ~ 1000r/min.
3. a kind of preparation method of visible light-responded nitrating nanometer titanium dioxide photochemical catalyst according to claim 1,
It is characterized in that：The inert gas is nitrogen or argon gas, and roasting vacuum degree by regulation and control and prepare has different colours and performance
Titania powder.
4. a kind of purposes of visible light-responded nitrogen-doped nanometer titanium dioxide catalyst described in claim 1, it is characterised in that：
Water is catalytically decomposed for the purification at air and water source, automatically cleaning, sun photodegradation water or solar photoelectric in the material.
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