CN108609650A - A kind of preparation method of nano-titanium dioxide - Google Patents
A kind of preparation method of nano-titanium dioxide Download PDFInfo
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 50
- 235000019441 ethanol Nutrition 0.000 claims abstract description 35
- 239000006185 dispersion Substances 0.000 claims abstract description 34
- 229920000609 methyl cellulose Polymers 0.000 claims abstract description 28
- 239000001923 methylcellulose Substances 0.000 claims abstract description 28
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 27
- 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 27
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 27
- 239000010936 titanium Substances 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 25
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 25
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 24
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000002186 photoactivation Effects 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000001879 gelation Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 25
- 239000004408 titanium dioxide Substances 0.000 abstract description 8
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 235000010981 methylcellulose Nutrition 0.000 description 24
- 230000001699 photocatalysis Effects 0.000 description 11
- 235000013339 cereals Nutrition 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 150000004040 pyrrolidinones Chemical class 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- PTHCMJGKKRQCBF-UHFFFAOYSA-N Cellulose, microcrystalline Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC)C(CO)O1 PTHCMJGKKRQCBF-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation 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
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- YLGXILFCIXHCMC-JHGZEJCSSA-N methyl cellulose Chemical compound COC1C(OC)C(OC)C(COC)O[C@H]1O[C@H]1C(OC)C(OC)C(OC)OC1COC YLGXILFCIXHCMC-JHGZEJCSSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 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
- 230000004044 response Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 235000009566 rice Nutrition 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
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to technical field of nano material, and in particular to tetrabutyl titanate is added into absolute ethyl alcohol 20 40min of ultrasonic disperse, obtains titanium alcohol liquid by a kind of preparation method of titanium dioxide, including step 1；Step 2, polyvinylpyrrolidone is added and is stirred into titanium alcohol liquid to being completely dissolved, then sealed 1 3h of ultrasonic reaction, obtain titanium alcohol dispersion liquid；Step 3, constant temperature is added into water in methylcellulose to stir to being completely dissolved, obtains aqueous dispersion；Step 4,2 4h of ultrasonic reaction is slowly added dropwise into titanium alcohol dispersion liquid in aqueous dispersion, obtains mixing micro- turbid；Step 5, micro- turbid will be mixed constant temperature is added into reaction kettle and stirred to gelation, and then filtered and use absolute ethyl alcohol constant temp while hot, obtain gel；Step 6, gel is put into ethanol water progress 1 3h of ultrasonic reaction, after filtering ultraviolet photoactivation obtain nano-titanium dioxide.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of preparation method of titanium dioxide.
Background technology
Currently as the TiO of one of semiconductor light-catalyst2Catalysis material is a kind of Novel ring of current most study
Border friendly materials, the property of photochemical catalyst are the key factors in Photocatalytic Oxidation.TiO2Crystal form, grain size and grain
The factors such as diameter, surface state have larger impact to its photocatalysis performance.The big nano-particle of surface area due to its skin effect and
Bulk effect determines that it has good catalytic activity and selectivity.Nano-TiO2Since its quantum size effect makes it lead
Band and valence-band level become discrete energy levels, and energy gap broadens, and conduction band current potential becomes more negative, and the corrigendum that valence band current potential becomes, this meaning
It with stronger oxidation and reducing power；Again because the grain size of nano-particle is small, photo-generated carrier more holds than coarse granule
Easily surface is moved to from inside particles, hence it is evident that reduce electronics and the recombination probability in hole, be also beneficial to improve photocatalysis performance.
Therefore, the small TiO of large specific surface area, grain size is prepared2Have 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, while titanium dioxide change of size is very big,
Photocatalysis performance is unstable.
Invention content
For the problems of the prior art, the present invention provides a kind of preparation method of nano-titanium dioxide, passes through polyethylene
Double dispersed encapsulated systems of pyrrolidones and methylcellulose complete the control that tetrabutyl titanate is converted into nano-titanium dioxide, no
The grain size of nano-titanium dioxide can be only controlled, while reducing reaction difficulty.
To realize the above technical purpose, the technical scheme is that：
A kind of preparation method of nano-titanium dioxide, includes the following steps：
Step 1, ultrasonic disperse 20-40min is added into absolute ethyl alcohol in tetrabutyl titanate, obtains titanium alcohol liquid；
Step 2, polyvinylpyrrolidone is added and is stirred into titanium alcohol liquid to being completely dissolved, then seal ultrasonic reaction 1-
3h obtains titanium alcohol dispersion liquid；
Step 3, constant temperature is added into water in methylcellulose to stir to being completely dissolved, obtains aqueous dispersion；
Step 4, the ultrasonic reaction 2-4h into titanium alcohol dispersion liquid is slowly added dropwise in aqueous dispersion, obtains mixing micro- turbid；
Step 5, micro- turbid will be mixed constant temperature is added into reaction kettle and stirred to gelation, then filtered while hot and use nothing
Water-ethanol constant temp, obtains gel；
Step 6, gel is put into ethanol water progress ultrasonic reaction 1-3h, after filtering ultraviolet photoactivation obtain nanometer
Titanium dioxide.
A concentration of 20-50g/L of the tetrabutyl titanate in absolute ethyl alcohol in the step 1.
The supersonic frequency of ultrasonic disperse in the step 1 is 20-30kHz, and temperature is 40-60 DEG C.
The addition of polyvinylpyrrolidone in the step 2 is the 70-80% of tetrabutyl titanate quality, the stirring
It is 1000-2000r/min to the mixing speed being completely dissolved.
The temperature of sealing ultrasonic reaction in the step 2 is 50-60 DEG C, supersonic frequency 25-35kHz.
The addition of methylcellulose in the step 3 is the 60-70% of tetrabutyl titanate quality, the Methyl cellulose
A concentration of 30-70g/L of element in water, the mixing speed of the constant temperature stirring is 2000-3000r/min, temperature 40-45
℃。
The rate of addition being slowly added dropwise in the step 4 is 2-5mL/min, and the supersonic frequency of the ultrasonic reaction is
20-25kHz。
The temperature of constant temperature stirring in the step 5 is 70-75 DEG C, mixing speed 1500-2500r/min, described to take advantage of
The temperature of heat filtering is 65-75 DEG C, and the temperature of the constant temp is 60-70 DEG C.
The ethyl alcohol volumetric concentration of ethanol water in the step 6 is 60-70%, and the gel is in ethanol water
A concentration of 20-30g/L, the supersonic frequency of the ultrasonic reaction is 40-90kHz, and temperature is 30-40 DEG C.
The ultraviolet ray intensity of ultraviolet photoactivation in the step 6 is 1.5-4.5mW/cm2。
Tetrabutyl titanate is dissolved in absolute ethyl alcohol by step 1 by the way of ultrasound, formation titanium alcohol liquid, and ultrasound
Clutch can fast vibration absolute ethyl alcohol, achieve the effect that rapid dispersion, while preventing its tetrabutyl titanate slow because dissolving
And it is deposited on bottom.
Polyvinylpyrrolidone is added into absolute ethyl alcohol step 2, can quickly be dissolved to be formed in absolute ethyl alcohol and divide
Alcohol system is dissipated, and stable micro- thick solution can be formed, tetrabutyl titanate is reacted with polyvinylpyrrolidone, can be in metatitanic acid table
Face forms stable polyvinylpyrrolidone clad structure, not only improves the dispersion of metatitanic acid, but also covered effect can
The fast hydrolyzing of metatitanic acid is prevented, hydrolysis rate is reduced.
Methylcellulose is carried out constant temperature stirring by step 3 into the water, and methyl fibre is promoted in the way of slightly heating
The solute effect of element is tieed up, and using the dispersing characteristic of methylcellulose and micro- consistence, the water with dispersion effect can be formed
Solution.
Aqueous dispersion is slowly added dropwise into titanium alcohol dispersion liquid and is carried out ultrasonic reaction by step 4, in the reaction system
Interior, the polyvinylpyrrolidone on metatitanic acid surface can be wrapped up shell rupture by ultrasonic reaction, and hydrone forms hydrolysis with metatitanic acid
Obtain nano-titania particle, the exposed nano-titania particle of formation is in methylcellulose and polyvinylpyrrolidone
Under double dispersing molecule effects, surface forms the dispersion of package structure, ensure that the good dispersion of nano-particle, prevents from receiving
The reunion of rice corpuscles；Polyvinylpyrrolidone in water with all have good dissolubility in absolute ethyl alcohol, can ensure metatitanic acid
The stability of particle in water, can control the progress of hydrolysis, and ultrasonic reaction condition destroys the packet of polyvinylpyrrolidone
System is wrapped up in, the flow that metatitanic acid hydrolyzes successively can be formed, achievees the purpose that control hydrolysis.
Step 5 will mix micro- turbid constant temperature in reaction kettle and stir, can be by methyl fibre by the heating in whipping process
Dimension element is converted into gel, and nano-titanium dioxide is formed dispersion consolidated structures, and polyvinylpyrrolidone can be converted into second
Alcohol dissolves；Stirring normal form can in ethanol by the constantly dissolving of cured polyvinylpyrrolidone reduce the continuous fragmentation of gel
Polyvinylpyrrolidone in gel；Nano-titanium dioxide and gel are retained in filter process while hot, removal contains polyethylene
The ethanol water of pyrrolidones, obtained precipitation is mainly based on nano-titanium dioxide and methyl cellulose gel, to solve
Polyvinylpyrrolidone impurity carries out constant temp using absolute ethyl alcohol, can not only be molten by water and polyvinylpyrrolidone
Solution in water, while can ensure that methylcellulose keeps gel state, finally obtain the gel containing nano-titanium dioxide.
Gel is put into ethanol water by step 6, and methylcellulose re-dissolves to form dispersion, at this time nanometer two
Titania surface is wrapped up with methylcellulose, reaches dispersion；Ultrasonic reaction destroys the package of methylcellulose, and from
Conjunction forms surface passivation under capable of acting on, reduce from reunion；It is handled using ultraviolet photoactivation after filtering, is existed using nano-titanium dioxide
Under ultraviolet light can response characteristic by the activation of nano-titanium dioxide, promote the photocatalytic activity of nano-titanium dioxide.
From the above, it can be seen that the present invention has following advantages：
1. the present invention completes tetrabutyl titanate by double dispersed encapsulated systems of polyvinylpyrrolidone and methylcellulose
It is converted into the control of nano-titanium dioxide, the grain size of nano-titanium dioxide can not only be controlled, while reducing reaction difficulty.
2. the present invention is hydrolyzed to main means to control, while reducing the chemical reaction between compound, improve poly-
The recycling possibility of vinylpyrrolidone and methylcellulose reduces environmental pollution and environmental protection treatment pressure.
3. titanium dioxide odorlessness prepared by the present invention, neutral, stability is good.The present invention has work compared with the prior art
Simple, the at low cost and high product purity remarkable advantage of skill.
Specific implementation mode
The present invention will be described in detail in conjunction with the embodiments, but does not do any restriction to the claim of the present invention.
Embodiment 1
A kind of preparation method of nano-titanium dioxide, includes the following steps：
Step 1, ultrasonic disperse 20min is added into absolute ethyl alcohol in tetrabutyl titanate, obtains titanium alcohol liquid；
Step 2, polyvinylpyrrolidone is added into titanium alcohol liquid and is stirred to being completely dissolved, then seal ultrasonic reaction
1h obtains titanium alcohol dispersion liquid；
Step 3, constant temperature is added into water in methylcellulose to stir to being completely dissolved, obtains aqueous dispersion；
Step 4, the ultrasonic reaction 2h into titanium alcohol dispersion liquid is slowly added dropwise in aqueous dispersion, obtains mixing micro- turbid；
Step 5, micro- turbid will be mixed constant temperature is added into reaction kettle and stirred to gelation, then filtered while hot and use nothing
Water-ethanol constant temp, obtains gel；
Step 6, gel is put into ethanol water progress ultrasonic reaction 1h, after filtering ultraviolet photoactivation obtain nanometer two
Titanium oxide.
A concentration of 20g/L of the tetrabutyl titanate in absolute ethyl alcohol in the step 1.
The supersonic frequency of ultrasonic disperse in the step 1 is 20kHz, and temperature is 40 DEG C.
The addition of polyvinylpyrrolidone in the step 2 is the 70% of tetrabutyl titanate quality, and the stirring is extremely
The mixing speed being completely dissolved is 1000r/min.
The temperature of sealing ultrasonic reaction in the step 2 is 50 DEG C, supersonic frequency 25kHz.
The addition of methylcellulose in the step 3 is the 60% of tetrabutyl titanate quality, the methylcellulose
The mixing speed of a concentration of 30g/L in water, the constant temperature stirring are 2000r/min, and temperature is 40 DEG C.
The rate of addition being slowly added dropwise in the step 4 is 2mL/min, and the supersonic frequency of the ultrasonic reaction is
20kHz。
The temperature of constant temperature stirring in the step 5 is 70 DEG C, mixing speed 1500r/min, described to filter while hot
Temperature is 65 DEG C, and the temperature of the constant temp is 60 DEG C.
The ethyl alcohol volumetric concentration of ethanol water in the step 6 is 60%, and the gel is in ethanol water
The supersonic frequency of a concentration of 20g/L, the ultrasonic reaction are 40kHz, and temperature is 30 DEG C.
The ultraviolet ray intensity of ultraviolet photoactivation in the step 6 is 1.5mW/cm2。
Embodiment 2
A kind of preparation method of nano-titanium dioxide, includes the following steps：
Step 1, ultrasonic disperse 40min is added into absolute ethyl alcohol in tetrabutyl titanate, obtains titanium alcohol liquid；
Step 2, polyvinylpyrrolidone is added into titanium alcohol liquid and is stirred to being completely dissolved, then seal ultrasonic reaction
3h obtains titanium alcohol dispersion liquid；
Step 3, constant temperature is added into water in methylcellulose to stir to being completely dissolved, obtains aqueous dispersion；
Step 4, the ultrasonic reaction 4h into titanium alcohol dispersion liquid is slowly added dropwise in aqueous dispersion, obtains mixing micro- turbid；
Step 5, micro- turbid will be mixed constant temperature is added into reaction kettle and stirred to gelation, then filtered while hot and use nothing
Water-ethanol constant temp, obtains gel；
Step 6, gel is put into ethanol water progress ultrasonic reaction 3h, after filtering ultraviolet photoactivation obtain nanometer two
Titanium oxide.
A concentration of 50g/L of the tetrabutyl titanate in absolute ethyl alcohol in the step 1.
The supersonic frequency of ultrasonic disperse in the step 1 is 30kHz, and temperature is 60 DEG C.
The addition of polyvinylpyrrolidone in the step 2 is the 80% of tetrabutyl titanate quality, and the stirring is extremely
The mixing speed being completely dissolved is 2000r/min.
The temperature of sealing ultrasonic reaction in the step 2 is 60 DEG C, supersonic frequency 35kHz.
The addition of methylcellulose in the step 3 is the 70% of tetrabutyl titanate quality, the methylcellulose
The mixing speed of a concentration of 70g/L in water, the constant temperature stirring are 3000r/min, and temperature is 45 DEG C.
The rate of addition being slowly added dropwise in the step 4 is 5mL/min, and the supersonic frequency of the ultrasonic reaction is
25kHz。
The temperature of constant temperature stirring in the step 5 is 75 DEG C, mixing speed 2500r/min, described to filter while hot
Temperature is 75 DEG C, and the temperature of the constant temp is 70 DEG C.
The ethyl alcohol volumetric concentration of ethanol water in the step 6 is 70%, and the gel is in ethanol water
The supersonic frequency of a concentration of 30g/L, the ultrasonic reaction are 90kHz, and temperature is 40 DEG C.
The ultraviolet ray intensity of ultraviolet photoactivation in the step 6 is 4.5mW/cm2。
Embodiment 3
A kind of preparation method of nano-titanium dioxide, includes the following steps：
Step 1, ultrasonic disperse 30min is added into absolute ethyl alcohol in tetrabutyl titanate, obtains titanium alcohol liquid；
Step 2, polyvinylpyrrolidone is added into titanium alcohol liquid and is stirred to being completely dissolved, then seal ultrasonic reaction
2h obtains titanium alcohol dispersion liquid；
Step 3, constant temperature is added into water in methylcellulose to stir to being completely dissolved, obtains aqueous dispersion；
Step 4, the ultrasonic reaction 3h into titanium alcohol dispersion liquid is slowly added dropwise in aqueous dispersion, obtains mixing micro- turbid；
Step 5, micro- turbid will be mixed constant temperature is added into reaction kettle and stirred to gelation, then filtered while hot and use nothing
Water-ethanol constant temp, obtains gel；
Step 6, gel is put into ethanol water progress ultrasonic reaction 2h, after filtering ultraviolet photoactivation obtain nanometer two
Titanium oxide.
A concentration of 35g/L of the tetrabutyl titanate in absolute ethyl alcohol in the step 1.
The supersonic frequency of ultrasonic disperse in the step 1 is 25kHz, and temperature is 50 DEG C.
The addition of polyvinylpyrrolidone in the step 2 is the 75% of tetrabutyl titanate quality, and the stirring is extremely
The mixing speed being completely dissolved is 1500r/min.
The temperature of sealing ultrasonic reaction in the step 2 is 55 DEG C, supersonic frequency 30kHz.
The addition of methylcellulose in the step 3 is the 65% of tetrabutyl titanate quality, the methylcellulose
The mixing speed of a concentration of 50g/L in water, the constant temperature stirring are 2500r/min, and temperature is 43 DEG C.
The rate of addition being slowly added dropwise in the step 4 is 3mL/min, and the supersonic frequency of the ultrasonic reaction is
23kHz。
The temperature of constant temperature stirring in the step 5 is 73 DEG C, mixing speed 2000r/min, described to filter while hot
Temperature is 70 DEG C, and the temperature of the constant temp is 65 DEG C.
The ethyl alcohol volumetric concentration of ethanol water in the step 6 is 65%, and the gel is in ethanol water
The supersonic frequency of a concentration of 25g/L, the ultrasonic reaction are 70kHz, and temperature is 35 DEG C.
The ultraviolet ray intensity of ultraviolet photoactivation in the step 6 is 3.5mW/cm2。
Performance detection
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example | |
| Grain size | 200nm | 300nm | 210nm | 700nm |
| Grain size concentrates ratio | 90% | 92% | 95% | 79% |
| Photocatalytic activity | 99% | 98% | 100% | 87% |
| Sterilizing rate | 99% | 99% | 99% | 99% |
| Stability | 95% | 96% | 98% | 81% |
Example is compared with embodiment by contrast, and there is catalysis material prepared by the present invention good photocatalysis stability to exist
95% or more, photocatalysis removal rate is 98% or more, higher than in comparative example 875% photocatalysis removal rate and 81% photocatalysis it is steady
It is qualitative.
In conclusion the present invention has the following advantages：
1. the present invention completes tetrabutyl titanate by double dispersed encapsulated systems of polyvinylpyrrolidone and methylcellulose
It is converted into the control of nano-titanium dioxide, the grain size of nano-titanium dioxide can not only be controlled, while reducing reaction difficulty.
2. the present invention is hydrolyzed to main means to control, while reducing the chemical reaction between compound, improve poly-
The recycling possibility of vinylpyrrolidone and methylcellulose reduces environmental pollution and environmental protection treatment pressure.
3. titanium dioxide odorlessness prepared by the present invention, neutral, stability is good.The present invention has work compared with the prior art
Simple, the at low cost and high product purity remarkable advantage of skill.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
Technical solution described in inventive embodiments.It will be understood by those of ordinary skill in the art that still can be carried out to the present invention
Modification or equivalent replacement, to reach identical technique effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of preparation method of nano-titanium dioxide, it is characterised in that：Include the following steps：
Step 1, ultrasonic disperse 20-40min is added into absolute ethyl alcohol in tetrabutyl titanate, obtains titanium alcohol liquid；
Step 2, polyvinylpyrrolidone is added and is stirred into titanium alcohol liquid to being completely dissolved, then seal ultrasonic reaction 1-3h,
Obtain titanium alcohol dispersion liquid；
Step 3, constant temperature is added into water in methylcellulose to stir to being completely dissolved, obtains aqueous dispersion；
Step 4, the ultrasonic reaction 2-4h into titanium alcohol dispersion liquid is slowly added dropwise in aqueous dispersion, obtains mixing micro- turbid；
Step 5, micro- turbid will be mixed constant temperature is added into reaction kettle and stirred to gelation, then filtered while hot and use anhydrous second
Alcohol constant temp, obtains gel；
Step 6, gel is put into ethanol water progress ultrasonic reaction 1-3h, after filtering ultraviolet photoactivation obtain nano-silica
Change titanium.
2. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 1
A concentration of 20-50g/L of the tetrabutyl titanate in absolute ethyl alcohol.
3. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 1
The supersonic frequency of ultrasonic disperse is 20-30kHz, and temperature is 40-60 DEG C.
4. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 2
The addition of polyvinylpyrrolidone is the 70-80% of tetrabutyl titanate quality, the stirring to the mixing speed being completely dissolved
For 1000-2000r/min.
5. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 2
The temperature for sealing ultrasonic reaction is 50-60 DEG C, supersonic frequency 25-35kHz.
6. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 3
The addition of methylcellulose is the 60-70% of tetrabutyl titanate quality, a concentration of 30- of the methylcellulose in water
The mixing speed of 70g/L, the constant temperature stirring are 2000-3000r/min, and temperature is 40-45 DEG C.
7. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 4
The rate of addition being slowly added dropwise is 2-5mL/min, and the supersonic frequency of the ultrasonic reaction is 20-25kHz.
8. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 5
The temperature of constant temperature stirring is 70-75 DEG C, mixing speed 1500-2500r/min, and the temperature filtered while hot is 65-75 DEG C,
The temperature of the constant temp is 60-70 DEG C.
9. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 6
The ethyl alcohol volumetric concentration of ethanol water is 60-70%, a concentration of 20-30g/L of the gel in ethanol water, described
The supersonic frequency of ultrasonic reaction is 40-90kHz, and temperature is 30-40 DEG C.
10. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 6
The ultraviolet ray intensity of ultraviolet photoactivation is 1.5-4.5mW/cm2。
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| CN109205667A (en) * | 2018-11-08 | 2019-01-15 | 绍兴文理学院 | A kind of preparation method of nano-titanium dioxide |
| CN109205664A (en) * | 2018-11-08 | 2019-01-15 | 绍兴文理学院 | A kind of method that electrostatic spinning prepares nano-titanium dioxide |
| CN109205666A (en) * | 2018-11-08 | 2019-01-15 | 绍兴文理学院 | A kind of high temperature preparation method of nano-titanium dioxide |
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| CN101333002A (en) * | 2007-06-27 | 2008-12-31 | 中国科学院合肥物质科学研究院 | Titanium dioxide nano powder with special morphology and preparation method thereof |
| CN106976907A (en) * | 2017-04-27 | 2017-07-25 | 吴亚良 | A kind of nano titanium oxide preparation method of size tunable |
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| CN101333002A (en) * | 2007-06-27 | 2008-12-31 | 中国科学院合肥物质科学研究院 | Titanium dioxide nano powder with special morphology and preparation method thereof |
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| CN109205667A (en) * | 2018-11-08 | 2019-01-15 | 绍兴文理学院 | A kind of preparation method of nano-titanium dioxide |
| CN109205664A (en) * | 2018-11-08 | 2019-01-15 | 绍兴文理学院 | A kind of method that electrostatic spinning prepares nano-titanium dioxide |
| CN109205666A (en) * | 2018-11-08 | 2019-01-15 | 绍兴文理学院 | A kind of high temperature preparation method of nano-titanium dioxide |
| CN109205666B (en) * | 2018-11-08 | 2021-06-15 | 绍兴文理学院 | High-temperature preparation method of nano titanium dioxide |
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