CN108483490A - 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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- CN108483490A CN108483490A CN201810278555.0A CN201810278555A CN108483490A CN 108483490 A CN108483490 A CN 108483490A CN 201810278555 A CN201810278555 A CN 201810278555A CN 108483490 A CN108483490 A CN 108483490A
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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 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 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 42
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 235000019441 ethanol Nutrition 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 28
- 239000002270 dispersing agent Substances 0.000 claims abstract description 20
- 239000004094 surface-active agent Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims abstract description 13
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 208000030208 low-grade fever Diseases 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims abstract description 11
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000012263 liquid product Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 2
- 229910052719 titanium Inorganic materials 0.000 claims 2
- 239000010936 titanium Substances 0.000 claims 2
- 241000790917 Dioxys <bee> Species 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 230000009471 action Effects 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229920002521 macromolecule Polymers 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
- 239000000047 product Substances 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 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
- 238000004821 distillation Methods 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
- 230000006872 improvement Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 239000000693 micelle 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
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 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
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 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
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
-
- 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)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to environment-friendly materials technical fields, and in particular to step 1 a kind of preparation method of nano-titanium dioxide tetrabutyl titanate is added into absolute ethyl alcohol, dispersant ultrasonic disperse is then added to being completely dissolved, and obtains tetrabutyl titanate dispersion alcohol liquid；Step 2, high molecular surfactant is added into distilled water, is evenly stirred until and is completely dissolved, obtain dropping liquid；Step 3, dropping liquid is slowly added dropwise into tetrabutyl titanate alcohol liquid, sealing low-grade fever stirs 1 3h, obtains suspension；Step 4, suspension is put into 1 3h of vacuum distillation reaction in reaction kettle, filter at low temperature obtains a coated titanium dioxide precipitation after cooling；Step 5,10 20min of ultrasonic reaction in ethanol water is added in coated titanium dioxide precipitation, then takes out high temperature drying, obtains nano-titanium dioxide.The present invention is hydrolyzed by tetrabutyl titanate, and using the double action of polyvinylpyrrolidone and lauryl sodium sulfate, can be formed good dispersion, be prevented the reunion of titanium dioxide.
Description
Technical field
The invention belongs to environment-friendly materials technical fields, and in particular to a kind of preparation method of nano-titanium dioxide.
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
For the problems of the prior art, the present invention provides a kind of preparation method of nano-titanium dioxide, just through pertitanic acid
Butyl ester hydrolyzes, and using the double action of polyvinylpyrrolidone and lauryl sodium sulfate, can form good dispersion
System prevents the reunion of titanium dioxide.
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, tetrabutyl titanate is added into absolute ethyl alcohol, dispersant ultrasonic disperse is then added to being completely dissolved,
Obtain tetrabutyl titanate dispersion alcohol liquid；
Step 2, high molecular surfactant is added into distilled water, is evenly stirred until and is completely dissolved, obtain dropping liquid；
Step 3, dropping liquid is slowly added dropwise into tetrabutyl titanate alcohol liquid, sealing low-grade fever stirs 1-3h, obtains suspension；
Step 4, suspension is put into vacuum distillation reaction 1-3h in reaction kettle, filter at low temperature obtains a coated after cooling
Titanium dioxide precipitation；
Step 5, ultrasonic reaction 10-20min in ethanol water is added in coated titanium dioxide precipitation, then takes out height
Temperature drying, obtains nano-titanium dioxide.
A concentration of 20-40g/L of the tetrabutyl titanate in absolute ethyl alcohol in the step 1.
Dispersant in the step 1 uses polyvinylpyrrolidone, and the addition of the dispersant is tetrabutyl titanate
The supersonic frequency of the 30-40% of quality, the ultrasonic disperse are 5-15kHz, and temperature is 50-60 DEG C.
A concentration of 90-150g/L of the high molecular surfactant in distilled water in the step 2, the high molecular form
It is 2000-3000r/min that face activating agent, which uses lauryl sodium sulfate, the mixing speed stirred evenly,.
The speed that is slowly added dropwise that dropping liquid in the step 3 is added into tetrabutyl titanate alcohol liquid is 2-5mL/min, institute
The temperature for stating sealing low-grade fever stirring is 70-80 DEG C, pressure 0.5-0.8MPa, and the speed of the stirring is 1000-2000r/
min。
The pressure of vacuum distillation reaction in the step 4 is the 70-80% of atmospheric pressure, and temperature is 80-90 DEG C, described to subtract
Volume after pressure distillation is the 20-30% of tetrabutyl titanate alcohol liquid product.
The temperature of filter at low temperature in the step 4 is 2-5 DEG C.
A concentration of 20-40g/L of coated titanium dioxide in the solution in the step 5, the ethanol water
Ethyl alcohol volumetric concentration is 40-80%.
The supersonic frequency of ultrasonic reaction in the step 5 is 10-20kHz, and temperature is 40-60 DEG C.
The temperature of high temperature drying in the step 5 is 300-350 DEG C.
Tetrabutyl titanate is added into absolute ethyl alcohol step 1, is aided with dispersant and forms dispersion, and in ultrasonic item
Under part, relatively stable structure is formed, polyvinylpyrrolidone can be dissolved in formation hemi-micelle structure in absolute ethyl alcohol, can
Form stable tetrabutyl titanate dispersion.
High molecular surfactant can be dissolved in distilled water by step 2, and being formed has good dispersion solution.
Dropping liquid is added into alcohol liquid step 3 can form tetrabutyl titanate slow hydrolysis, form low grain size at this time
Titanium dioxide granule, and adhere to the package characteristic of dispersing characteristic and dispersant on the surface of high molecular surfactant, it can
Form suspension；
Step 4 is removed the absolute ethyl alcohol in suspension by the way of vacuum distillation, is improved hydrolysis efficiency, is deposited simultaneously
It is acted in high molecular surfactant and dispersant, nano-titanium dioxide is wrapped up, solves the problems, such as titanium dioxide reunion.
Step 5 carries out ultrasonic disperse using ethanol water, can be dissolved high molecular surfactant using distilled water,
Achieve the purpose that removal, while the peptizaiton of dispersant and surfactant, will not only form reunion, but also can be by two
Titanium oxide dispersion is suspended；It is anatase titanium dioxide by the transformation of crystal of titanium dioxide finally under high temperature drying condition；It is water-soluble using ethyl alcohol
Liquid can make full use of the good film forming of ethyl alcohol, promote whole colloidal property, form the dispersion effect of different systems, effectively
Solve agglomeration traits, while also solving the agglomeration traits in pure aquatic system, greatly promote the stability of grain size.
From the above, it can be seen that the present invention has following advantages：
1. the present invention is hydrolyzed by tetrabutyl titanate, and utilizes pair of polyvinylpyrrolidone and lauryl sodium sulfate
Recast is used, and can be formed good dispersion, be prevented the reunion of titanium dioxide.
2. catalysis material prepared by the present invention has good photocatalysis stability 98% or more, photocatalysis removes
Rate is 90% or more.
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.
4. the present invention can effectively control the grain size of nano-titanium dioxide, together using polyvinylpyrrolidone as coating agent
When using lauryl sodium sulfate as surface action agent, the agglomeration traits generated when coating agent removes can be prevented.
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, tetrabutyl titanate is added into absolute ethyl alcohol, dispersant ultrasonic disperse is then added to being completely dissolved,
Obtain tetrabutyl titanate dispersion alcohol liquid；
Step 2, high molecular surfactant is added into distilled water, is evenly stirred until and is completely dissolved, obtain dropping liquid；
Step 3, dropping liquid is slowly added dropwise into tetrabutyl titanate alcohol liquid, sealing low-grade fever stirs 1h, obtains suspension；
Step 4, suspension is put into vacuum distillation reaction 1h in reaction kettle, filter at low temperature obtains a coated two after cooling
Titanium oxide precipitate；
Step 5, ultrasonic reaction 10min in ethanol water is added in coated titanium dioxide precipitation, then takes out high temperature
Drying, obtains nano-titanium dioxide.
A concentration of 20g/L of the tetrabutyl titanate in absolute ethyl alcohol in the step 1.
Dispersant in the step 1 uses polyvinylpyrrolidone, and the addition of the dispersant is tetrabutyl titanate
The supersonic frequency of the 30% of quality, the ultrasonic disperse is 5kHz, and temperature is 50 DEG C.
A concentration of 90g/L of the high molecular surfactant in distilled water in the step 2, the macromolecule surface are lived
Property agent use lauryl sodium sulfate, the mixing speed stirred evenly be 2000r/min.
The speed that is slowly added dropwise that dropping liquid in the step 3 is added into tetrabutyl titanate alcohol liquid is 2mL/min, described
The temperature for sealing low-grade fever stirring is 70 DEG C, pressure 0.5MPa, and the speed of the stirring is 1000r/min.
The pressure of vacuum distillation reaction in the step 4 is the 70% of atmospheric pressure, and temperature is 80 DEG C, the vacuum distillation
Volume afterwards is the 20% of tetrabutyl titanate alcohol liquid product.
The temperature of filter at low temperature in the step 4 is 2 DEG C.
A concentration of 20g/L of coated titanium dioxide in the solution in the step 5, the ethyl alcohol of the ethanol water
Volumetric concentration is 40%.
The supersonic frequency of ultrasonic reaction in the step 5 is 10kHz, and temperature is 40 DEG C.
The temperature of high temperature drying in the step 5 is 300 DEG C.
Gained titanium dioxide is white, and crystal form is anatase titanium dioxide, and odorlessness, neutral, stability is good, and grain size is 800nm or so.
Embodiment 2
A kind of preparation method of nano-titanium dioxide, includes the following steps：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, dispersant ultrasonic disperse is then added to being completely dissolved,
Obtain tetrabutyl titanate dispersion alcohol liquid；
Step 2, high molecular surfactant is added into distilled water, is evenly stirred until and is completely dissolved, obtain dropping liquid；
Step 3, dropping liquid is slowly added dropwise into tetrabutyl titanate alcohol liquid, sealing low-grade fever stirs 3h, obtains suspension；
Step 4, suspension is put into vacuum distillation reaction 3h in reaction kettle, filter at low temperature obtains a coated two after cooling
Titanium oxide precipitate；
Step 5, ultrasonic reaction 20min in ethanol water is added in coated titanium dioxide precipitation, then takes out high temperature
Drying, obtains nano-titanium dioxide.
A concentration of 40g/L of the tetrabutyl titanate in absolute ethyl alcohol in the step 1.
Dispersant in the step 1 uses polyvinylpyrrolidone, and the addition of the dispersant is tetrabutyl titanate
The supersonic frequency of the 40% of quality, the ultrasonic disperse is 15kHz, and temperature is 60 DEG C.
A concentration of 150g/L of the high molecular surfactant in distilled water in the step 2, the macromolecule surface
It is 3000r/min that activating agent, which uses lauryl sodium sulfate, the mixing speed stirred evenly,.
The speed that is slowly added dropwise that dropping liquid in the step 3 is added into tetrabutyl titanate alcohol liquid is 5mL/min, described
The temperature for sealing low-grade fever stirring is 80 DEG C, pressure 0.8MPa, and the speed of the stirring is 2000r/min.
The pressure of vacuum distillation reaction in the step 4 is the 80% of atmospheric pressure, and temperature is 90 DEG C, the vacuum distillation
Volume afterwards is the 30% of tetrabutyl titanate alcohol liquid product.
The temperature of filter at low temperature in the step 4 is 5 DEG C.
A concentration of 40g/L of coated titanium dioxide in the solution in the step 5, the ethyl alcohol of the ethanol water
Volumetric concentration is 80%.
The supersonic frequency of ultrasonic reaction in the step 5 is 20kHz, and temperature is 60 DEG C.
The temperature of high temperature drying in the step 5 is 350 DEG C.
Gained titanium dioxide is white, and crystal form is anatase titanium dioxide, and odorlessness, neutral, stability is good, and grain size is 500nm or so.
Embodiment 3
A kind of preparation method of nano-titanium dioxide, includes the following steps：
Step 1, tetrabutyl titanate is added into absolute ethyl alcohol, dispersant ultrasonic disperse is then added to being completely dissolved,
Obtain tetrabutyl titanate dispersion alcohol liquid；
Step 2, high molecular surfactant is added into distilled water, is evenly stirred until and is completely dissolved, obtain dropping liquid；
Step 3, dropping liquid is slowly added dropwise into tetrabutyl titanate alcohol liquid, sealing low-grade fever stirs 2h, obtains suspension；
Step 4, suspension is put into vacuum distillation reaction 2h in reaction kettle, filter at low temperature obtains a coated two after cooling
Titanium oxide precipitate；
Step 5, ultrasonic reaction 15min in ethanol water is added in coated titanium dioxide precipitation, then takes out high temperature
Drying, obtains nano-titanium dioxide.
A concentration of 30g/L of the tetrabutyl titanate in absolute ethyl alcohol in the step 1.
Dispersant in the step 1 uses polyvinylpyrrolidone, and the addition of the dispersant is tetrabutyl titanate
The supersonic frequency of the 30-40% of quality, the ultrasonic disperse are 10kHz, and temperature is 55 DEG C.
A concentration of 120g/L of the high molecular surfactant in distilled water in the step 2, it is described to stir evenly
Mixing speed is 2500r/min.
The speed that is slowly added dropwise that dropping liquid in the step 3 is added into tetrabutyl titanate alcohol liquid is 4mL/min, described
The temperature for sealing low-grade fever stirring is 75 DEG C, pressure 0.6MPa, and the speed of the stirring is 1500r/min.
The pressure of vacuum distillation reaction in the step 4 is the 75% of atmospheric pressure, and temperature is 85 DEG C, the vacuum distillation
Volume afterwards is the 25% of tetrabutyl titanate alcohol liquid product.
The temperature of filter at low temperature in the step 4 is 4 DEG C.
A concentration of 30g/L of coated titanium dioxide in the solution in the step 5, the ethyl alcohol of the ethanol water
Volumetric concentration is 60%.
The supersonic frequency of ultrasonic reaction in the step 5 is 15kHz, and temperature is 50 DEG C.
The temperature of high temperature drying in the step 5 is 330 DEG C.
Gained titanium dioxide is white, and crystal form is anatase titanium dioxide, and odorlessness, neutral, stability is good, and grain size is 150nm or so.
Performance test
Using GB/T 23762-2009 (catalysis material water solution system purifies test method) as the property of catalysis material
Energy detection method, as a comparison case with P25, contrast properties test is as follows：
In conclusion the present invention has the following advantages：
1. the present invention is hydrolyzed by tetrabutyl titanate, and utilizes pair of polyvinylpyrrolidone and lauryl sodium sulfate
Recast is used, and can be formed good dispersion, be prevented the reunion of titanium dioxide.
2. catalysis material prepared by the present invention has good photocatalysis stability 98% or more, photocatalysis removes
Rate is 90% or more.
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.
4. the present invention can effectively control the grain size of nano-titanium dioxide, together using polyvinylpyrrolidone as coating agent
When using lauryl sodium sulfate as surface action agent, the agglomeration traits generated when coating agent removes can be prevented.
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, tetrabutyl titanate is added into absolute ethyl alcohol, dispersant ultrasonic disperse is then added to being completely dissolved, obtains
Tetrabutyl titanate disperses alcohol liquid；
Step 2, high molecular surfactant is added into distilled water, is evenly stirred until and is completely dissolved, obtain dropping liquid；
Step 3, dropping liquid is slowly added dropwise into tetrabutyl titanate alcohol liquid, sealing low-grade fever stirs 1-3h, obtains suspension；
Step 4, suspension is put into vacuum distillation reaction 1-3h in reaction kettle, filter at low temperature obtains a coated dioxy after cooling
Change titanium precipitation；
Step 5, ultrasonic reaction 10-20min in ethanol water is added in coated titanium dioxide precipitation, then takes out high temperature baking
It is dry, obtain nano-titanium dioxide.
2. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：Titanium in the step 1
A concentration of 20-40g/L of the sour N-butyl 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
Dispersant uses polyvinylpyrrolidone, and the addition of the dispersant is the 30-40% of tetrabutyl titanate quality, the ultrasound
The supersonic frequency of dispersion is 5-15kHz, and temperature is 50-60 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
A concentration of 90-150g/L of the high molecular surfactant in distilled water, the high molecular surfactant use dodecyl
Sodium sulphate, the mixing speed stirred evenly are 2000-3000r/min.
5. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 3
The speed that is slowly added dropwise that dropping liquid is added into tetrabutyl titanate alcohol liquid is 2-5mL/min, the temperature of the sealing low-grade fever stirring
It it is 70-80 DEG C, the speed of pressure 0.5-0.8MPa, the stirring are 1000-2000r/min.
6. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 4
The pressure of vacuum distillation reaction is the 70-80% of atmospheric pressure, and temperature is 80-90 DEG C, and the volume after the vacuum distillation is metatitanic acid
The 20-30% of N-butyl alcohol liquid product.
7. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 4
The temperature of filter at low temperature is 2-5 DEG C.
8. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 5
The ethyl alcohol volumetric concentration of a concentration of 20-40g/L of coated titanium dioxide in the solution, the ethanol water are 40-80%.
9. a kind of preparation method of nano-titanium dioxide according to claim 1, it is characterised in that：In the step 5
The supersonic frequency of ultrasonic reaction is 10-20kHz, and temperature is 40-60 DEG C.
10. 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 high temperature drying is 300-350 DEG C.
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| CN109399688A (en) * | 2018-10-17 | 2019-03-01 | 贵州芭田生态工程有限公司 | The method of phosphate fertilizer mother liquor low temperature decalcification and decalcification filtrate and phosphate fertilizer preparation method |
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| CN114736664A (en) * | 2022-05-26 | 2022-07-12 | 西南石油大学 | Nano titanium dioxide solid particle emulsifier and preparation method thereof |
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| CN109264778A (en) * | 2018-10-16 | 2019-01-25 | 张静娟 | A kind of preparation method of the nano-titanium dioxide of size tunable |
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| CN109205666B (en) * | 2018-11-08 | 2021-06-15 | 绍兴文理学院 | High-temperature preparation method of nano titanium dioxide |
| CN109626421A (en) * | 2018-12-06 | 2019-04-16 | 浙江离火新材料科技有限公司 | The preparation method for the titanium dioxide nanoparticle that organic film coats completely |
| CN114736664A (en) * | 2022-05-26 | 2022-07-12 | 西南石油大学 | Nano titanium dioxide solid particle emulsifier and preparation method thereof |
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