CN106976907A - A kind of nano titanium oxide preparation method of size tunable - Google Patents
A kind of nano titanium oxide preparation method of size tunable Download PDFInfo
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- CN106976907A CN106976907A CN201710284378.2A CN201710284378A CN106976907A CN 106976907 A CN106976907 A CN 106976907A CN 201710284378 A CN201710284378 A CN 201710284378A CN 106976907 A CN106976907 A CN 106976907A
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- tetrabutyl titanate
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 47
- 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 abstract description 30
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 24
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 24
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 23
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000007789 sealing Methods 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000010992 reflux Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 55
- 238000005292 vacuum distillation Methods 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 10
- 238000005286 illumination Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 230000036647 reaction Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 230000006641 stabilisation Effects 0.000 claims description 5
- 238000011105 stabilization Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000004408 titanium dioxide Substances 0.000 abstract description 17
- 239000002245 particle Substances 0.000 abstract description 16
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- 238000007146 photocatalysis Methods 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000006056 electrooxidation reaction Methods 0.000 abstract description 2
- 230000005281 excited state Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 9
- 238000006555 catalytic reaction Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- 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
-
- B01J35/39—
-
- B01J35/40—
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- 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
- C02F2305/08—Nanoparticles or nanotubes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a kind of nano titanium oxide preparation method of size tunable, sealing reaction is carried out using polyvinylpyrrolidone and tetrabutyl titanate and water bath sonicator reaction obtains white semigel, and add normal heptane and carry out heating reflux reaction and obtain milky suspension, finally by milky suspension after carrying out the anatase titanium dioxide that micro-current and photo-irradiation treatment obtain excited state twice.Titanium dioxide particle diameter prepared by this method is controlled by the ratio of tetrabutyl titanate and polyvinylpyrrolidone, while having ensured the particle diameter of titanium dioxide using the covered effect of polyvinylpyrrolidone；The titanium dioxide particle diameter distribution that simultaneously prepared by this method is uniform, and photocatalysis performance is notable, and electrochemical corrosion resistant effect is good.
Description
Technical field
The invention belongs to catalysis material technical field, and in particular to a kind of nano titanium oxide preparation side of size tunable
Method.
Background technology
It is used as the TiO of one of semiconductor light-catalyst2Catalysis material is a kind of novel environmental friend of current most study
Good material, the property of photochemical catalyst is the key factor in Photocatalytic Oxidation.TiO2Crystal formation, grain size and particle diameter,
The factors such as surface state have considerable influence to its photocatalysis performance.The big nano-particle of surface area is due to its skin effect and volume
Effect, determines that it has good catalytic activity and selectivity.Nano-TiO2Due to its quantum size effect make its conduction band and
Valence-band level becomes discrete energy levels, and energy gap broadens, and it is more negative that conduction band current potential becomes, and the corrigendum that valence band current potential becomes, it means that its
With stronger oxidation and reducing power；Again because nano-particle particle diameter it is small, photo-generated carrier than coarse granule be more prone to from
Inside particles move to surface, hence it is evident that reduce electronics and the recombination probability in hole, are also beneficial to improve photocatalysis performance.Cause
This, prepares the TiO that specific surface area is big, particle diameter is small2Turn into the focus of photocatalysis field research.
As the improvement of people's living standards, environmentally conscious materialses are more paid close attention to by people, titanium dioxide optical catalyst tool
There are the excellent properties such as oxidation activity is high, catalytic performance is strong, activity stabilized, moisture resistance is good and sterilizing ability is strong, in wastewater degradation, disappear
It is widely used in terms of removing and harmful gas, sterilization and purification air.But the preparation side of existing titanium dioxide powder
Method, such as traditional solid phase reaction and sintering process and modern chemical vapour deposition technique, physical vaporous deposition, chemical vapor infiltration
Method, sol-gel processing etc., these methods have the shortcomings that complex process, cost are high, resulting often mixing crystal formation and
Granularity is uneven, because the Photocatalytic activity of rutile titanium dioxide and unformed titanium dioxide is very poor.
The content of the invention
The purpose of the present invention is that there is provided a kind of nano titanium oxide system of size tunable in view of the deficiencies of the prior art
Preparation Method, the catalysis material of preparation has stable photocatalysis effect, while also having good structural soundness, Yi Jixing
Stabilizability, and with good electrocorrosion-resisting performance..
In order to solve the above-mentioned technical problem, the present invention provides a kind of nano titanium oxide preparation method of size tunable, its
Comprise the following steps that：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, then adds polyvinylpyrrolidone, sealed after stirring
React 2-5h, natural cooling；
Step 2, the reaction solution of step 1 is subjected to vacuum distillation reaction, obtains faint yellow sol solutionses；
Step 3, sol solutionses are used into ethanol washing by soaking, then water bath sonicator reaction 10-15min, depressurizes and steam after natural cooling
Evaporate to form white semigel；
Step 4, white semigel is added and stirred in normal heptane, then heating reflux reaction 2-5h, obtained milky and hang
Turbid liquid；
Step 5, after milky suspension is filtered, micro-current electroanalysis processing and photo-irradiation treatment are carried out, you can obtain anatase titanium dioxide two
Titanium oxide.
Absolute ethyl alcohol addition in step 1 is 10-15 times of tetrabutyl titanate quality, and the polyvinylpyrrolidone is
4-8 times of tetrabutyl titanate, the mixing speed is 500-1500r/min, and the sealing reaction pressure is 1.3-3.5MPa；Should
Tetrabutyl titanate is dispersed in absolute ethyl alcohol by step, can form tetrabutyl titanate weak solution, polyvinylpyrrolidone is in second
Dissolved in alcohol, stable micro- thick solution can be formed, it is anti-by the tetrabutyl titanate in absolute ethyl alcohol and polyvinylpyrrolidone
Should, stable polyvinylpyrrolidone clad structure is formed on metatitanic acid surface.
The pressure of vacuum distillation in step 2 is the 15-35% of atmospheric pressure, and the vapo(u)rizing temperature is 70-80 DEG C；In decompression
In still-process, absolute ethyl alcohol rapid evaporation, while the N-butyl carried in tetrabutyl titanate is also progressively evaporated, so as to form poly-
Vinylpyrrolidone wraps up the thick alcohol liquid of titanium dioxide.
The quality of ethanol in step 3 is 4-8 times of tetrabutyl titanate, and the water bath sonicator temperature is 50-65 DEG C, described
Supersonic frequency is 10-15min, and the pressure of the vacuum distillation is the 50-70% of atmospheric pressure, and the vapo(u)rizing temperature is 60-70 DEG C；
By the dissolving of ethanol, and water bath sonicator is carried out, the cladding played between destruction polyvinylpyrrolidone and metatitanic acid is connected, and this surpasses
Phonoresponse produces clutch energy, destroys valence bond structure, secondary polyvinylpyrrolidone parcel is finally carried out during rotary evaporation,
Package structure is more explained more fully.
Normal heptane addition in step 4 is 3-5 times of tetrabutyl titanate, and the sealing back flow reaction temperature is 70-80 DEG C,
While normal heptane and ethanol are dissolved, polyvinylpyrrolidone is dissolved in ethanol, will during sealing back flow reaction
Normal heptane is acted on to metatitanic acid surface, coating reaction is destroyed, while metatitanic acid is separated out into white graininess, because W-response is in
In absolute ethyl alcohol system, metatitanic acid dehydration forms titanium dioxide granule, and keeps particle diameter under normal heptane effect, prevents cluster of grains
It is poly-.
Micro-current electroanalysis reaction in step 5 uses current stabilization cell reaction, and electric current is 3-8A, and the electrolyte concentration is
0.3-0.8mol/L, micro-current electroanalysis reaction time 3-6h；Fast speed heat burning effect can be played by the way of light electrolysis
Really, the normal heptane of titanium dioxide surface is removed in the way of thermal diffusion and electrolysis and degradation, while forming sharp under electrolytic condition
Titanium-type structure.
Photo-irradiation treatment in step 5 uses UV illumination, and the uviol lamp requirement is 365nm, during the photo-irradiation treatment
Between be 2-5h, the illumination temperature is not higher than 50 DEG C；Photo-irradiation treatment can activate the photocatalysis performance of anatase titanium dioxide.
The present invention carries out sealing reaction by using polyvinylpyrrolidone and tetrabutyl titanate and reacted with water bath sonicator
To white semigel, and add normal heptane carry out heating reflux reaction obtain milky suspension, finally by milky suspension
The anatase titanium dioxide of excited state is obtained with photo-irradiation treatment after progress micro-current twice.Titanium dioxide grain prepared by this method
Footpath is controlled by the ratio of tetrabutyl titanate and polyvinylpyrrolidone, while being imitated using the cladding of polyvinylpyrrolidone
Fruit has ensured the particle diameter of titanium dioxide；The titanium dioxide particle diameter distribution that simultaneously prepared by this method is uniform, and photocatalysis performance is notable, and
Electrochemical corrosion resistant effect is good.
Compared with prior art, the invention has the advantages that：
（1）The nano titanium oxide prepared in the present invention is to wrap up system by the polyvinylpyrrolidone of titanium dioxide hydrolyzation system
It is standby, with good and consistent particle diameter, it can be convenient to use in actual production.
（2）Catalysis material prepared by the present invention has stable photocatalysis effect, while also having good structure steady
Solidity, and stability, and with good electrocorrosion-resisting performance.
（3）Titanium dioxide odorlessness prepared by the present invention, neutral, stability is good.The present invention has compared with the prior art
Technique is simple, cost is low and the high remarkable advantage of product purity.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the titanic oxide material prepared by embodiment 1.
Embodiment
The present invention is described further with reference to embodiment：
Embodiment 1
A kind of nano titanium oxide preparation method of size tunable, it is comprised the following steps that：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, then adds polyvinylpyrrolidone, sealed after stirring
React 2h, natural cooling；
Step 2, the reaction solution of step 1 is subjected to vacuum distillation reaction, obtains faint yellow sol solutionses；
Step 3, sol solutionses are used into ethanol washing by soaking, then water bath sonicator reaction 10min, vacuum distillation shape after natural cooling
Into white semigel；
Step 4, white semigel is added and stirred in normal heptane, then heating reflux reaction 2h, obtains milky suspended
Liquid；
Step 5, after milky suspension is filtered, micro-current electroanalysis processing and photo-irradiation treatment are carried out, you can obtain anatase titanium dioxide two
Titanium oxide.
Absolute ethyl alcohol addition in step 1 is 10 times of tetrabutyl titanate quality, and the polyvinylpyrrolidone is titanium
4 times of sour N-butyl, the mixing speed is 500r/min, and the sealing reaction pressure is 1.3MPa.
The pressure of vacuum distillation in step 2 is the 15% of atmospheric pressure, and the vapo(u)rizing temperature is 70 DEG C.
The quality of ethanol in step 3 is 4 times of tetrabutyl titanate, and the water bath sonicator temperature is 50 DEG C, the ultrasound
Frequency is 10min, and the pressure of the vacuum distillation is the 50% of atmospheric pressure, and the vapo(u)rizing temperature is 60 DEG C.
Normal heptane addition in step 4 is 3 times of tetrabutyl titanate, and the sealing back flow reaction temperature is 70 DEG C.
Micro-current electroanalysis reaction in step 5 uses current stabilization cell reaction, and electric current is 3A, and the electrolyte concentration is
0.3mol/L, micro-current electroanalysis reaction time 3h.
Photo-irradiation treatment in step 5 uses UV illumination, and the uviol lamp requirement is 365nm, during the photo-irradiation treatment
Between be 2h, the illumination temperature be 50 DEG C.
Gained titanium dioxide is white, and crystal formation is anatase titanium dioxide, and odorlessness is neutral, and stability is good.Its scanning electron microscope (SEM) photograph is as schemed
1, particle diameter is 300nm or so.
Embodiment 2
A kind of nano titanium oxide preparation method of size tunable, it is comprised the following steps that：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, then adds polyvinylpyrrolidone, sealed after stirring
React 5h, natural cooling；
Step 2, the reaction solution of step 1 is subjected to vacuum distillation reaction, obtains faint yellow sol solutionses；
Step 3, sol solutionses are used into ethanol washing by soaking, then water bath sonicator reaction 15min, vacuum distillation shape after natural cooling
Into white semigel；
Step 4, white semigel is added and stirred in normal heptane, then heating reflux reaction 5h, obtains milky suspended
Liquid；
Step 5, after milky suspension is filtered, micro-current electroanalysis processing and photo-irradiation treatment are carried out, you can obtain anatase titanium dioxide two
Titanium oxide.
Absolute ethyl alcohol addition in step 1 is 15 times of tetrabutyl titanate quality, and the polyvinylpyrrolidone is titanium
8 times of sour N-butyl, the mixing speed is 1500r/min, and the sealing reaction pressure is 3.5MPa.
The pressure of vacuum distillation in step 2 is the 35% of atmospheric pressure, and the vapo(u)rizing temperature is 80 DEG C.
The quality of ethanol in step 3 is 8 times of tetrabutyl titanate, and the water bath sonicator temperature is 65 DEG C, the ultrasound
Frequency is 15min, and the pressure of the vacuum distillation is the 70% of atmospheric pressure, and the vapo(u)rizing temperature is 70 DEG C.
Normal heptane addition in step 4 is 5 times of tetrabutyl titanate, and the sealing back flow reaction temperature is 80 DEG C.
Micro-current electroanalysis reaction in step 5 uses current stabilization cell reaction, and electric current is 8A, and the electrolyte concentration is
0.8mol/L, micro-current electroanalysis reaction time 6h.
Photo-irradiation treatment in step 5 uses UV illumination, and the uviol lamp requirement is 365nm, during the photo-irradiation treatment
Between be 5h, the illumination temperature be 30 DEG C.
Gained titanium dioxide is white, and crystal formation is anatase titanium dioxide, and odorlessness is neutral, and stability is good, and particle diameter is 15nm or so.
Embodiment 3
A kind of nano titanium oxide preparation method of size tunable, it is comprised the following steps that：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, then adds polyvinylpyrrolidone, sealed after stirring
React 3h, natural cooling；
Step 2, the reaction solution of step 1 is subjected to vacuum distillation reaction, obtains faint yellow sol solutionses；
Step 3, sol solutionses are used into ethanol washing by soaking, then water bath sonicator reaction 13min, vacuum distillation shape after natural cooling
Into white semigel；
Step 4, white semigel is added and stirred in normal heptane, then heating reflux reaction 4h, obtains milky suspended
Liquid；
Step 5, after milky suspension is filtered, micro-current electroanalysis processing and photo-irradiation treatment are carried out, you can obtain anatase titanium dioxide two
Titanium oxide.
Absolute ethyl alcohol addition in step 1 is 13 times of tetrabutyl titanate quality, and the polyvinylpyrrolidone is titanium
6 times of sour N-butyl, the mixing speed is 1100r/min, and the sealing reaction pressure is 2.4MPa.
The pressure of vacuum distillation in step 2 is the 25% of atmospheric pressure, and the vapo(u)rizing temperature is 75 DEG C.
The quality of ethanol in step 3 is 6 times of tetrabutyl titanate, and the water bath sonicator temperature is 55 DEG C, the ultrasound
Frequency is 13min, and the pressure of the vacuum distillation is the 60% of atmospheric pressure, and the vapo(u)rizing temperature is 65 DEG C.
Normal heptane addition in step 4 is 4 times of tetrabutyl titanate, and the sealing back flow reaction temperature is 75 DEG C.
Micro-current electroanalysis reaction in step 5 uses current stabilization cell reaction, and electric current is 5A, and the electrolyte concentration is
0.6mol/L, micro-current electroanalysis reaction time 5h.
Photo-irradiation treatment in step 5 uses UV illumination, and the uviol lamp requirement is 365nm, during the photo-irradiation treatment
Between be 3h, the illumination temperature be 40 DEG C.
Gained titanium dioxide is white, and crystal formation is anatase titanium dioxide, and odorlessness is neutral, and stability is good, and particle diameter is 200nm or so.
Embodiment 4
With GB/T 23762-2009（Catalysis material water solution system purifies method of testing）Examined as the performance of catalysis material
Survey method, experiment is compared with embodiment 1 and comparative example.
Comparative example uses the pure titinium dioxide photochemical catalyst of same particle size.
Embodiment and the impact of performance that comparative example handles methylene blue waste liquid are as follows：
| Embodiment 1 | Comparative example | |
| Particle diameter | 300nm | 300nm |
| Quality | 10g | 10g |
| Photocatalysis clearance | 90% | 67% |
| Photocatalysis stability | 98% | 87% |
Example is compared with embodiment 1 by contrast, and catalysis material prepared by the present invention has good photocatalysis stability 98%
More than, photocatalysis clearance is more than 90%, higher than the 75% photocatalysis clearance and 90% photocatalysis stability in comparative example.
One embodiment of the invention is the foregoing is only, the present invention, all use equivalent substitutions or equivalent transformation is not intended to limit
The technical scheme that is obtained of mode, all fall within protection scope of the present invention.
Claims (7)
1. a kind of nano titanium oxide preparation method of size tunable, it is comprised the following steps that：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, then adds polyvinylpyrrolidone, sealed after stirring
React 2-5h, natural cooling；
Step 2, the reaction solution of step 1 is subjected to vacuum distillation reaction, obtains faint yellow sol solutionses；
Step 3, sol solutionses are used into ethanol washing by soaking, then water bath sonicator reaction 10-15min, depressurizes and steam after natural cooling
Evaporate to form white semigel；
Step 4, white semigel is added and stirred in normal heptane, then heating reflux reaction 2-5h, obtained milky and hang
Turbid liquid；
Step 5, after milky suspension is filtered, micro-current electroanalysis processing and photo-irradiation treatment are carried out, you can obtain anatase titanium dioxide two
Titanium oxide.
2. a kind of nano titanium oxide preparation method of size tunable according to claim 1, it is characterised in that step 1
In absolute ethyl alcohol addition be 10-15 times of tetrabutyl titanate quality, the polyvinylpyrrolidone is tetrabutyl titanate
4-8 times, the mixing speed is 500-1500r/min, and the sealing reaction pressure is 1.3-3.5MPa.
3. a kind of nano titanium oxide preparation method of size tunable according to claim 1, it is characterised in that step 2
In vacuum distillation pressure be atmospheric pressure 15-35%, the vapo(u)rizing temperature be 70-80 DEG C.
4. a kind of nano titanium oxide preparation method of size tunable according to claim 1, it is characterised in that step 3
In the quality of ethanol be 4-8 times of tetrabutyl titanate, the water bath sonicator temperature is 50-65 DEG C, and the supersonic frequency is 10-
15min, the pressure of the vacuum distillation is the 50-70% of atmospheric pressure, and the vapo(u)rizing temperature is 60-70 DEG C.
5. a kind of nano titanium oxide preparation method of size tunable according to claim 1, it is characterised in that step 4
In normal heptane addition be 3-5 times of tetrabutyl titanate, the sealing back flow reaction temperature is 70-80 DEG C.
6. a kind of nano titanium oxide preparation method of size tunable according to claim 1, it is characterised in that step 5
In micro-current electroanalysis reaction use current stabilization cell reaction, electric current is 3-8A, the electrolyte concentration be 0.3-0.8mol/L, institute
State micro-current electroanalysis reaction time 3-6h.
7. a kind of nano titanium oxide preparation method of size tunable according to claim 1, it is characterised in that step 5
In photo-irradiation treatment use UV illumination, the uviol lamp requirement is 365nm, and the photo-irradiation treatment time is 2-5h, described
Illumination temperature is not higher than 50 DEG C.
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