CN106976907B - A kind of nano-titanium dioxide preparation method of size tunable - Google Patents
A kind of nano-titanium dioxide preparation method of size tunable Download PDFInfo
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- CN106976907B CN106976907B CN201710284378.2A CN201710284378A CN106976907B CN 106976907 B CN106976907 B CN 106976907B CN 201710284378 A CN201710284378 A CN 201710284378A CN 106976907 B CN106976907 B CN 106976907B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 67
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 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
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 23
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 23
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 23
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 22
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 44
- 235000019441 ethanol Nutrition 0.000 claims description 16
- 238000007789 sealing Methods 0.000 claims description 15
- 238000005292 vacuum distillation Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 10
- 238000005286 illumination Methods 0.000 claims description 10
- 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
- 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 8
- 239000002245 particle Substances 0.000 abstract description 5
- 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
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000010992 reflux Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 10
- 238000006555 catalytic reaction Methods 0.000 description 7
- 239000002253 acid Substances 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
- 230000008569 process 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
- 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
- 239000007788 liquid 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
- 230000001954 sterilising effect Effects 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000002604 ultrasonography Methods 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
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 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
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007596 consolidation process Methods 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
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004821 distillation 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
- -1 polyethylene Pyrrolidones Polymers 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
- 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
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- 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
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- 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
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Abstract
The invention discloses a kind of nano-titanium dioxide preparation methods of size tunable, it is sealed to react with tetrabutyl titanate using polyvinylpyrrolidone and white semigel is obtained by the reaction with water bath sonicator, and normal heptane progress heating reflux reaction is added and obtains milky suspension, milky suspension is finally obtained into the anatase titanium dioxide of excited state after progress micro-current twice with photo-irradiation treatment.Titanium dioxide grain size prepared by this method is controlled by the ratio of tetrabutyl titanate and polyvinylpyrrolidone, while the grain size of titanium dioxide has been ensured 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 fields, and in particular to a kind of nano-titanium dioxide preparation side of size tunable
Method.
Background technology
TiO as one of semiconductor light-catalyst2Catalysis material is a kind of novel environmental friend of current most study
Good material, the property of photochemical catalyst are the key factors in Photocatalytic Oxidation.TiO2Crystal form, grain size and grain size,
The factors such as surface state have larger impact 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 conduction band current potential becomes more negative, and the corrigendum that valence band current potential becomes, it means that its
With stronger oxidation and reducing power；Again because nano-particle grain size 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, be also beneficial to improve photocatalysis performance.Cause
This, prepares the small TiO of large specific surface area, grain size2Have become the focus of photocatalysis field research.
As the improvement of people's living standards, environmentally conscious materials are more paid close attention to by people, titanium dioxide optical catalyst tool
Have that oxidation activity is high, catalytic performance is strong, activity stabilized, moisture resistance is good and the sterilizing ability excellent properties such as by force, in wastewater degradation, disappears
Removing and harmful gas, sterilization and purification air etc. are widely used.However 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, of high cost, obtained often mixing crystal form and
Granularity is uneven, because the Photocatalytic activity of rutile titanium dioxide and unformed titanium dioxide is very poor.
Invention content
The purpose of the present invention is in view of the deficiencies of the prior art, provide a kind of nano-titanium dioxide system of size tunable
The catalysis material of Preparation Method, preparation has stable photocatalysis effect, while also having good structural soundness, Yi Jixing
Stabilizability, and there is good electrocorrosion-resisting performance.
In order to solve the above technical problem, the present invention provides a kind of nano-titanium dioxide preparation method of size tunable,
It is as follows：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, polyvinylpyrrolidone is then added, after stirring evenly
Sealing reaction 2-5h, natural cooling；
Step 2, the reaction solution of step 1 is subjected to vacuum distillation reaction, obtains faint yellow sol solutions；
Step 3, sol solutions are used into ethyl alcohol washing by soaking, then water bath sonicator reacts 10-15min, subtracts after natural cooling
Pressure distillation forms white semigel；
Step 4, white semigel is added in normal heptane and is stirred evenly, then sealed back flow reaction 2-5h, obtain milky white
Color suspension；
Step 5, after milky suspension being filtered, micro-current electroanalysis processing and photo-irradiation treatment are carried out, you can obtain rutile titania
Type titanium dioxide.
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 are 500-1500r/min, and the sealing reaction pressure is 1.3-3.5MPa；It should
Tetrabutyl titanate is dispersed in absolute ethyl alcohol by step, can form tetrabutyl titanate weak solution, polyvinylpyrrolidone is in second
It is dissolved in alcohol, stable micro- thick solution can be formed, it is anti-by tetrabutyl titanate in absolute ethyl alcohol and polyvinylpyrrolidone
It answers, forms stable polyvinylpyrrolidone clad structure on metatitanic acid surface.
The pressure of vacuum distillation in step 2 is the 15-35% of atmospheric pressure, and vapo(u)rizing temperature is 70-80 DEG C；It is being evaporated under reduced pressure
In the process, absolute ethyl alcohol rapid evaporation, while the N-butyl carried in tetrabutyl titanate is also gradually evaporated, to form polyethylene
Pyrrolidones wraps up the thick alcohol liquid of titanium dioxide.
The quality of ethyl alcohol in step 3 is 4-8 times of tetrabutyl titanate, and the temperature of the water bath sonicator is 50-65 DEG C, is surpassed
Acoustic frequency is 10-15kHz, and the pressure of the vacuum distillation is the 50-70% of atmospheric pressure, and vapo(u)rizing temperature is 60-70 DEG C；Pass through second
The dissolving of alcohol, and water bath sonicator is carried out, it plays the cladding destroyed between polyvinylpyrrolidone and metatitanic acid and connects, the ultrasonic reaction
Clutch energy is generated, valence bond structure is destroyed, secondary polyvinylpyrrolidone package, package knot are finally carried out during rotary evaporation
Structure more consolidation is more fully.
Normal heptane addition in step 4 is tetrabutyl titanate de 3-5 times, and the sealing back flow reaction temperature is 70-80
DEG C, while normal heptane and ethyl alcohol are dissolved, polyvinylpyrrolidone is dissolved in ethyl alcohol, in sealing back flow reaction process
In, normal heptane is acted on to metatitanic acid surface, coating reaction is destroyed, while white graininess is precipitated in metatitanic acid, due to integral inverted
It should be in absolute ethyl alcohol system, metatitanic acid dehydration forms titanium dioxide granule, and keeps grain size under normal heptane effect, prevents
Particle agglomeration.
Micro-current electroanalysis reaction in step 5 uses current stabilization cell reaction, electric current 3-8A, electrolyte concentration 0.3-
0.8mol/L, the micro-current electroanalysis reaction time 3-6h；Fast speed heat combustion efficiency can be played by the way of light electrolysis, it will
The normal heptane of titanium dioxide surface is removed in a manner of thermal diffusion and electrolysis and degradation, while anatase titanium dioxide knot is formed under electrolytic condition
Structure.
Photo-irradiation treatment in step 5 uses UV illumination, and the ultraviolet lamp requires to be 365nm, when the photo-irradiation treatment
Between be 2-5h, the illumination temperature be not higher than 50 DEG C；Photo-irradiation treatment can activate the photocatalysis performance of anatase titanium dioxide.
The present invention is sealed to react by using polyvinylpyrrolidone with tetrabutyl titanate to react with water bath sonicator
To white semigel, and normal heptane progress heating reflux reaction is added and obtains milky suspension, finally by milky suspension
After carrying out micro-current twice the anatase titanium dioxide of excited state is obtained with photo-irradiation treatment.Titanium dioxide grain prepared by this method
Diameter is controlled by the ratio of tetrabutyl titanate and polyvinylpyrrolidone, while being imitated using the cladding of polyvinylpyrrolidone
Fruit has ensured the grain size 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) nano-titanium dioxide prepared in the present invention is the polyvinylpyrrolidone packet by titanium dioxide hydrolyzation system
It wraps up in and is prepared, there is good and consistent grain size, 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 there is 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
Remarkable advantage simple for process, at low cost and high product purity.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the titanic oxide material prepared by embodiment 1.
Specific implementation mode
The present invention is described further with reference to embodiment：
Embodiment 1
A kind of nano-titanium dioxide preparation method of size tunable, is as follows：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, polyvinylpyrrolidone is then added, after stirring evenly
Sealing reaction 2h, natural cooling；
Step 2, the reaction solution of step 1 is subjected to vacuum distillation reaction, obtains faint yellow sol solutions；
Step 3, sol solutions are used into ethyl alcohol washing by soaking, then water bath sonicator reacts 10min, depressurizes and steams after natural cooling
It evaporates to form white semigel；
Step 4, white semigel is added in normal heptane and is stirred evenly, then sealed back flow reaction 2h, obtain milky
Suspension；
Step 5, after milky suspension being filtered, micro-current electroanalysis processing and photo-irradiation treatment are carried out, you can obtain rutile titania
Type titanium dioxide.
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 are 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 ethyl alcohol in step 3 is 4 times of tetrabutyl titanate, and the water bath sonicator temperature is 50 DEG C, the ultrasound
Frequency is 10kHz, 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 in step 5 is reacted using current stabilization cell reaction, electric current 3A, and the electrolyte concentration is
0.3mol/L, the micro-current electroanalysis reaction time 3h.
Photo-irradiation treatment in step 5 uses UV illumination, and the ultraviolet lamp requires to be 365nm, when the photo-irradiation treatment
Between be 2h, the illumination temperature be 50 DEG C.
Gained titanium dioxide is white, and crystal form is anatase titanium dioxide, and odorlessness is neutral, and stability is good.Its scanning electron microscope (SEM) photograph is as schemed
1, grain size is 300nm or so.
Embodiment 2
A kind of nano-titanium dioxide preparation method of size tunable, is as follows：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, polyvinylpyrrolidone is then added, after stirring evenly
Sealing reaction 5h, natural cooling；
Step 2, the reaction solution of step 1 is subjected to vacuum distillation reaction, obtains faint yellow sol solutions；
Step 3, sol solutions are used into ethyl alcohol washing by soaking, then water bath sonicator reacts 15min, depressurizes and steams after natural cooling
It evaporates to form white semigel；
Step 4, white semigel is added in normal heptane and is stirred evenly, then sealed back flow reaction 5h, obtain milky
Suspension；
Step 5, after milky suspension being filtered, micro-current electroanalysis processing and photo-irradiation treatment are carried out, you can obtain rutile titania
Type titanium dioxide.
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 are 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 vapo(u)rizing temperature is 80 DEG C.
The quality of ethyl alcohol in step 3 is 8 times of tetrabutyl titanate, and the water bath sonicator temperature is 65 DEG C, the ultrasound
Frequency is 15kHz, 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, electric current 8A, electrolyte concentration 0.8mol/
L, the micro-current electroanalysis reaction time 6h.
Photo-irradiation treatment in step 5 uses UV illumination, and the ultraviolet lamp requires to be 365nm, when the photo-irradiation treatment
Between be 5h, the illumination temperature be 30 DEG C.
Gained titanium dioxide is white, and crystal form is anatase titanium dioxide, and odorlessness, neutral, stability is good, and grain size is 15nm or so.
Embodiment 3
A kind of nano-titanium dioxide preparation method of size tunable, is as follows：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, polyvinylpyrrolidone is then added, after stirring evenly
Sealing reaction 3h, natural cooling；
Step 2, the reaction solution of step 1 is subjected to vacuum distillation reaction, obtains faint yellow sol solutions；
Step 3, sol solutions are used into ethyl alcohol washing by soaking, then water bath sonicator reacts 13min, depressurizes and steams after natural cooling
It evaporates to form white semigel；
Step 4, white semigel is added in normal heptane and is stirred evenly, then sealed back flow reaction 4h, obtain milky
Suspension；
Step 5, after milky suspension being filtered, micro-current electroanalysis processing and photo-irradiation treatment are carried out, you can obtain rutile titania
Type titanium dioxide.
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 are 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 ethyl alcohol in step 3 is 6 times of tetrabutyl titanate, and the water bath sonicator temperature is 55 DEG C, supersonic frequency
For 13kHz, 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, electric current 5A, electrolyte concentration 0.6mol/
L, the micro-current electroanalysis reaction time 5h.
Photo-irradiation treatment in step 5 uses UV illumination, and the ultraviolet lamp requires to be 365nm, when the photo-irradiation treatment
Between be 3h, the illumination temperature be 40 DEG C.
Gained titanium dioxide is white, and crystal form is anatase titanium dioxide, and odorlessness, neutral, stability is good, and grain size is 200nm or so.
Embodiment 4
Using GB/T 23762-2009 (catalysis material water solution system purifies test method) as the property of catalysis material
Energy detection method, experiment is compared with comparative example with embodiment 1.
Comparative example uses the pure titinium dioxide photochemical catalyst of same particle size.
The impact of performance that embodiment handles methylene blue waste liquid with comparative example is as follows：
| Embodiment 1 | Comparative example | |
| Grain size | 300nm | 300nm |
| Quality | 10g | 10g |
| Photocatalysis removal rate | 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 equal
98% or more, photocatalysis removal rate is 90% or more, is higher than 75% photocatalysis removal rate in comparative example and 90% photocatalysis
Stability.
The foregoing is merely one embodiment of the invention, are not intended to limit the present invention, all to use equivalent substitution or equivalent transformation
The technical solution that is obtained of mode, all fall in protection scope of the present invention.
Claims (6)
1. a kind of nano-titanium dioxide preparation method of size tunable, it is characterised in that：It is as follows：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, polyvinylpyrrolidone is then added, sealed after stirring evenly
2-5h is reacted, natural cooling, the polyvinylpyrrolidone is 4-8 times of tetrabutyl titanate；
Step 2, the reaction solution of step 1 is subjected to vacuum distillation reaction, obtains faint yellow sol solutions；
Step 3, sol solutions are used into ethyl alcohol washing by soaking, then water bath sonicator reacts 10-15min, depressurizes and steams after natural cooling
It evaporates to form white semigel；
Step 4, white semigel being added in normal heptane and is stirred evenly, normal heptane dissolves to form absolute ethyl alcohol system with ethyl alcohol,
Then back flow reaction 2-5h is sealed, milky suspension is obtained；
Step 5, it after milky suspension being filtered, carries out micro-current electroanalysis processing and is handled with UV illumination, you can obtained sharp
Titanium-type titanium dioxide, the micro-current electroanalysis reaction are using current stabilization cell reaction, electric current 3-8A, the electrolyte concentration
0.3-0.8mol/L, the micro-current electroanalysis reaction time 3-6h.
2. a kind of nano-titanium dioxide preparation method of size tunable according to claim 1, which is characterized in that step 1
In absolute ethyl alcohol addition be 10-15 times of tetrabutyl titanate quality, the mixing speed is 500-1500r/min, described
Sealing reaction pressure is 1.3-3.5MPa.
3. a kind of nano-titanium dioxide preparation method of size tunable according to claim 1, which is characterized 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 dioxide preparation method of size tunable according to claim 1, which is characterized in that step 3
In the quality of ethyl alcohol be 4-8 times of tetrabutyl titanate, the water bath sonicator temperature is 50-65 DEG C, and the supersonic frequency is 10-
15kHz, the pressure of the vacuum distillation are the 50-70% of atmospheric pressure, and vapo(u)rizing temperature is 60-70 DEG C.
5. a kind of nano-titanium dioxide preparation method of size tunable according to claim 1, which is characterized 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 dioxide preparation method of size tunable according to claim 1, which is characterized in that step 5
In ultraviolet lamp require be 365nm, the photo-irradiation treatment time be 2-5h, illumination temperature be not higher than 50 DEG C.
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| CN108483490A (en) * | 2018-03-31 | 2018-09-04 | 蒋建华 | A kind of preparation method of nano-titanium dioxide |
| CN108659664A (en) * | 2018-04-13 | 2018-10-16 | 广东煌盛体育设施有限公司 | A kind of Novel pollution-free environmental protection coating material |
| CN108502923B (en) * | 2018-04-29 | 2020-11-20 | 绍兴市览海环保科技有限公司 | Preparation method of nano titanium dioxide material with uniform particle size distribution |
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| CN108609650B (en) * | 2018-06-06 | 2020-11-13 | 绍兴市秀臻新能源科技有限公司 | Preparation method of nano titanium dioxide |
| CN108751252B (en) * | 2018-06-07 | 2020-05-19 | 广西藤县广峰钛白有限公司 | Preparation method of titanium dioxide with controllable particle size |
| CN108993558A (en) * | 2018-08-13 | 2018-12-14 | 蒋黎婷 | A kind of preparation method of high-performance titanium dioxide optical catalyst |
| CN109179495B (en) * | 2018-08-28 | 2021-04-06 | 绍兴文理学院 | Preparation method of high-dispersion nano titanium dioxide |
| CN109126756A (en) * | 2018-08-28 | 2019-01-04 | 绍兴文理学院 | A kind of preparation method of high-activity nano titanium dioxide |
| CN109319834B (en) * | 2018-11-08 | 2021-01-26 | 绍兴文理学院 | Preparation method of nano titanium dioxide |
| CN110042494B (en) * | 2019-04-28 | 2021-10-29 | 闽江学院 | Functional fiber compounding process |
| CN114231055A (en) * | 2021-12-31 | 2022-03-25 | 广东粤港澳大湾区国家纳米科技创新研究院 | Modified nano titanium dioxide material and preparation method and application thereof |
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