CN107021522B - A kind of monodisperse TiO based on microemulsion2The synthetic method of microballoon - Google Patents
A kind of monodisperse TiO based on microemulsion2The synthetic method of microballoon Download PDFInfo
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- CN107021522B CN107021522B CN201710311743.4A CN201710311743A CN107021522B CN 107021522 B CN107021522 B CN 107021522B CN 201710311743 A CN201710311743 A CN 201710311743A CN 107021522 B CN107021522 B CN 107021522B
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- microballoon
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- butyl titanate
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- 238000010189 synthetic method Methods 0.000 title claims abstract description 11
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 37
- 150000001875 compounds Chemical class 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000006210 lotion Substances 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000002242 deionisation method Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000004005 microsphere Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 239000005416 organic matter Substances 0.000 claims 1
- 239000000839 emulsion Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 4
- 238000006482 condensation reaction Methods 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 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
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The present invention provides a kind of monodisperse mesoporous TiO based on microemulsion2The synthetic method of microballoon belongs to inorganic functional material preparation technical field.The stable tetra-n-butyl titanate complex compound of acetylacetone,2,4-pentanedione is dispersed in water, form the polydisperse system of similar lotion, it is separated in removal emulsion system after the dispersed oil droplets of a small amount of micron-scale by centrifugally operated, original opaque polydispersion emulsion system is changed into transparent microemulsion system.The hydro-thermal process for carrying out 150 DEG C to the microemulsion system is achieved with monodispersed mesoporous TiO2Microballoon.The changeable synthesized mesoporous TiO of microemulsion system is further diluted with water2The size of microballoon.
Description
Technical field
The invention belongs to inorganic functional material preparation technical fields, and in particular to monodisperse TiO2The synthetic method of microballoon.
Background technique
Semiconductor TiO2Because of stable, environmental-friendly, the low preparation cost of physicochemical properties and strong photocatalytic degradation
Ability is widely used in photochemical catalyst, dye-sensitized solar cells, lithium battery, antifog and self-cleaning surface material etc.
Research.TiO2The design of pattern and micro-structure has important influence for the performance of its performance.In the latest 20 years, monodisperse is situated between
The TiO of pore structure2Microballoon or its complex microsphere are because brilliant in dye-sensitized solar cells, lithium battery, photochemical catalyst and photon
Body etc. application and the concern by numerous researchers.Monodisperse mesoporous TiO2Microballoon is used as photochemical catalyst
When have the advantages that high adsorption capacity and convenient for recycling, as thin-film material in use, being conducive to improve the capture of photon
Efficiency can effectively improve the photoelectric conversion efficiency of dye-sensitized solar cells.Existing synthesis monodisperse TiO2The work of microballoon
Skill is often used organic solvent as decentralized medium, and needs that some special measures is taken such as to add surfactant, use
The ionic strength etc. that salt is added as template, in precursor solution to improve solution in other mono-dispersion microballoons.The present invention utilizes
The acetylacetone,2,4-pentanedione stable unique molecular structure of tetra-n-butyl titanate complex compound and mild hydrolysis properties, it is steady to be configured with thermodynamics
Fixed water-based microemulsion, this method using water as decentralized medium do not need that other special substances such as surfactant, work is added
Skill is simple, environmentally protective.Surface-active is not necessarily to when the stable tetra-n-butyl titanate complex compound of acetylacetone,2,4-pentanedione is dispersed in water
The interface stability effect of agent forms the dispersion of similar lotion, has just obtained appearance transparent by simple centrifugally operated
Microemulsion.By water-heat process, wherein the tetra-n-butyl titanate complex compound oil phase droplet dispersed mutually merges, undergoes hydrolysis-
Polycondensation reaction is converted into the monodispersed TiO with meso-hole structure2Microballoon.
Summary of the invention
The present invention is configured with its dispersion system using the stable tetra-n-butyl titanate complex compound of acetylacetone,2,4-pentanedione, then through letter
Single centrifugally operated has just obtained the thermodynamically stable microemulsion system of appearance transparent.By hydro-thermal process, disperse in micro emulsion
Tetra-n-butyl titanate complex compound oil phase droplet mutually merges, hydrolysis-condensation reaction is undergone to be converted into monodispersed TiO2Microballoon.
By the way that additional water is added in the microemulsion system to configuration, then carries out identical hydrothermal process also and can further adjust and is synthesized
TiO2The size of microballoon.The present invention provides a kind of monodisperse TiO based on microemulsion2The synthetic method of microballoon, this method is with water
As decentralized medium, it is environmentally protective other particular matters, the simple processes such as addition surfactant are not needed.
The present invention realizes above-mentioned monodisperse TiO2The technical solution of microballoon is: using acetylacetone,2,4-pentanedione to tetra-n-butyl titanate into
Row complexing to mitigate the too high hydrolysis rate of tetra-n-butyl titanate, be then dispersed in deionized water formed it is flaxen more
Dispersion, separating a small amount of brown polymer grease that removal is precipitated by centrifugally operated can be obtained transparent micro emulsion dispersion
System.In water-heat process, as the temperature rises, the small oil droplet that is dispersed in microemulsion system while physics and chemistry are undergone
Variation.On the one hand, the small oil droplet of dispersion mutually merges and is formed the oil droplet of larger size because of the decline of stability；Another party
Face, oil droplet are converted into mesoporous TiO because tetra-n-butyl titanate complex compound therein undergoes hydrolysis-condensation reaction2Microballoon.To Microsoft
Additional water is added in system can reinforce the hydrolysis-condensation reaction of small oil droplet at relatively low temperatures, accelerate mineralising and the surface of oil droplet
Hardening process, and then weaken the fusion phenomenon between oil droplet, to synthesize the monodisperse TiO of smaller size2Microballoon.The technology include with
Lower step:
1, the preparation of tetra-n-butyl titanate complex compound
Acetylacetone,2,4-pentanedione is mixed into tetra-n-butyl titanate in appropriate proportion, is stirred to react 0.5h, is obtaining metatitanic acid four just
Butyl ester complex compound.
2, the preparation of tetra-n-butyl titanate complex compound polydispersion emulsion system
In the case of stirring, tetra-n-butyl titanate complex compound is added in the deionized water of certain volume, stirring point
1h is dissipated, the water-based emulsion system of tetra-n-butyl titanate complex compound is obtained.
3, centrifugal treating
The polydispersion emulsion system that step 2 is obtained carries out centrifugally operated.After centrifugal treating, upper layer is transparent micro emulsion
A small amount of brown oil has been precipitated in liquid, bottom.It separates except oily precipitate, obtains transparent microemulsion.
4, hydro-thermal reaction
The micro emulsion dispersion is transferred in reaction kettle, after reacting 10h at 150 DEG C, cooled to room temperature.
5, it washs
After the sample that hydro-thermal reaction obtains is centrifuged, spends ion-cleaning, then with ethanol washing three times.
6, dry
Sample after washing dries 2h in 100 DEG C of baking oven.
7, it calcines
The sample of step (6) after dry is placed in Muffle furnace, in 550 DEG C of temperature lower calcination 1h, can be obtained single point
Scattered TiO2Microspheres product.
Detailed description of the invention
TiO corresponding to the various dispersion liquids of Fig. 12Microballoon SEM photograph；Wherein, (a) lotion (embodiment 1), (b) microemulsion
(embodiment 2) (c) adds 1 times of water-reducible microemulsion (embodiment 3), (d) adds 3 times of water-reducible microemulsions (embodiment 4).
TiO synthesized by Fig. 22The size of microballoon is distributed.(a), (b), (c) and (d) corresponding TiO2The average diameter of microballoon is
1.84,2.83,1.12 and 0.68 μm.
Specific embodiment
With specific embodiment, invention is further explained below.
Embodiment 1:
One, the preparation of tetra-n-butyl titanate complex compound
2mL acetylacetone,2,4-pentanedione is mixed into 5mL tetra-n-butyl titanate, 0.5h is stirred to react, obtains tetra-n-butyl titanate network
Close object.
Two, the preparation of tetra-n-butyl titanate complex dispersion
In the case of stirring, tetra-n-butyl titanate complex compound is added in the deionization of 40mL and is dispersed with stirring 1h, obtained
To the water-based emulsion of tetra-n-butyl titanate complex compound.
Three, hydro-thermal reaction
The emulsion dispersion system is transferred in ptfe autoclave, 10h is reacted at 150 DEG C, naturally cools to room
Temperature.
Four, it washs
After the sample that hydro-thermal reaction obtains is centrifuged, spends ion-cleaning, then with ethanol washing three times.
Five, dry
Sample after washing dries 2h in 100 DEG C of baking oven.
Six, it calcines
Sample of the step (5) after dry is placed in Muffle furnace, in 550 DEG C of temperature lower calcination 1h, can be obtained single point
Scattered TiO2Microspheres product.SEM photograph (Fig. 1 (a)) shows the non-uniform TiO of size2Microballoon.
Embodiment 2:
One, the preparation of tetra-n-butyl titanate complex compound
2mL acetylacetone,2,4-pentanedione is mixed into 5mL tetra-n-butyl titanate, 0.5h is stirred to react, obtains tetra-n-butyl titanate network
Close object.
Two, the preparation of tetra-n-butyl titanate complex dispersion
In the case of stirring, tetra-n-butyl titanate complex compound is added in the deionization of 40mL and is dispersed with stirring 1h, obtained
To the water-based emulsion of tetra-n-butyl titanate complex compound.
Three, centrifugal treating
Water-based emulsion is subjected to centrifugally operated, revolving speed: 4000 turns/min, the time: 6min.After centrifugal treating, upper layer is
A small amount of yellow oil has been precipitated in bright microemulsion, bottom.It separates except oily precipitate, obtains transparent microemulsion.
Four, hydro-thermal reaction
The microemulsion dispersion is transferred in ptfe autoclave, 10h is reacted at 150 DEG C, naturally cools to
Room temperature.
Five, it washs
After the sample that hydro-thermal reaction obtains is centrifuged, spends ion-cleaning, then with ethanol washing three times.
Six, dry
Sample after washing dries 2h in 100 DEG C of baking oven.
Seven, it calcines
Sample of the step (6) after dry is placed in Muffle furnace, in 550 DEG C of temperature lower calcination 1h, can be obtained single point
Scattered TiO2Microspheres product.SEM photograph (Fig. 1 (b)) shows TiO of uniform size2Microballoon.
Embodiment 3:
One, the preparation of tetra-n-butyl titanate complex compound
2mL acetylacetone,2,4-pentanedione is mixed into 5mL tetra-n-butyl titanate, 0.5h is stirred to react, obtains tetra-n-butyl titanate network
Close object.
Two, the preparation of tetra-n-butyl titanate complex dispersion
In the case of stirring, tetra-n-butyl titanate complex compound is added in the deionization of 40mL and is dispersed with stirring 1h, obtained
To the water-based emulsion of tetra-n-butyl titanate complex compound.
Three, centrifugal treating
Water-based emulsion is subjected to centrifugally operated, revolving speed: 4000 turns/min, the time: 6min.After centrifugal treating, upper layer is
A small amount of yellow oil has been precipitated in bright microemulsion, bottom.It separates except oily precipitate, obtains transparent microemulsion.
Four, it dilutes
Microemulsion is diluted to 2 times of original volume with deionization.
Five, hydro-thermal reaction
Microemulsion after dilution is transferred in ptfe autoclave, 10h is reacted at 150 DEG C, naturally cools to room
Temperature.
Six, it washs
After the sample that hydro-thermal reaction obtains is centrifuged, spends ion-cleaning, then with ethanol washing three times.
Seven, dry
Sample after washing dries 2h in 100 DEG C of baking oven.
Eight, it calcines
Sample of the step (7) after dry is placed in Muffle furnace, in 550 DEG C of temperature lower calcination 1h, can be obtained single point
Scattered TiO2Microspheres product.SEM photograph (Fig. 1 (c)) shows TiO of uniform size2Microballoon, compared with the product of embodiment 2, directly
Diameter is smaller.
Embodiment 4:
One, the preparation of tetra-n-butyl titanate complex compound
2mL acetylacetone,2,4-pentanedione is mixed into 5mL tetra-n-butyl titanate, 0.5h is stirred to react, obtains tetra-n-butyl titanate network
Close object.
Two, the preparation of tetra-n-butyl titanate complex dispersion
In the case of stirring, tetra-n-butyl titanate complex compound is added in the deionization of 40mL and is dispersed with stirring 1h, obtained
To the water-based emulsion of tetra-n-butyl titanate complex compound.
Three, centrifugal treating
Water-based emulsion is subjected to centrifugally operated, revolving speed: 4000 turns/min, the time: 6min.After centrifugal treating, upper layer is
A small amount of yellow oil has been precipitated in bright microemulsion, bottom.It separates except oily precipitate, obtains transparent microemulsion.
Four, it dilutes
Microemulsion is diluted to 4 times of original volume with deionization.
Five, hydro-thermal reaction
Microemulsion after dilution is transferred in ptfe autoclave, 10h is reacted at 150 DEG C, naturally cools to room
Temperature.
Six, it washs
After the sample that hydro-thermal reaction obtains is centrifuged, spends ion-cleaning, then with ethanol washing three times.
Seven, dry
Sample after washing dries 2h in 100 DEG C of baking oven.
Eight, it calcines
Sample of the step (7) after dry is placed in Muffle furnace, in 550 DEG C of temperature lower calcination 1h, can be obtained single point
Scattered TiO2Microspheres product.SEM photograph (Fig. 1 (d)) shows TiO of uniform size2Microballoon, diameter is smaller, but exists between microballoon
Agglomeration, the excessive dilution of this explanation accelerate the hydrolysis-condensation reaction of oil droplet, result in incomplete fusion phenomenon.
Claims (5)
1. a kind of monodisperse TiO based on microemulsion2The synthetic method of microballoon, it is characterised in that: the synthetic method includes following
Step:
(1), the preparation of tetra-n-butyl titanate complex compound
Acetylacetone,2,4-pentanedione is mixed into tetra-n-butyl titanate in proportion, is stirred to react 0.5h, obtains tetra-n-butyl titanate complex compound；
(2), the preparation of the aqueous polydispersion lotion of tetra-n-butyl titanate
In the case of stirring, the tetra-n-butyl titanate complex compound that step (1) obtains is added in the deionization of certain volume,
It is dispersed with stirring 1h, obtains the aqueous polydispersion lotion of tetra-n-butyl titanate complex compound；
(3), centrifugal treating
The aqueous polydispersion lotion that step (2) is obtained carries out centrifugally operated, revolving speed: 4000 turns/min, the time: 6min, centrifugation
After processing, upper layer is transparent microemulsion, and bottom has been precipitated a small amount of brown oil, has separated except oily precipitate, obtain
The transparent microemulsion in upper layer；
(4), hydro-thermal reaction
Microemulsion described in step (3) is transferred in reaction kettle, after reacting 10h at 150 DEG C, cooled to room temperature；
(5), it washs
After being centrifuged by the sample that step (4) hydro-thermal reaction obtains, spend ion-cleaning, then with ethanol washing three times；
(6) dry
Sample after step (5) washing is dried in baking oven；
(7) it calcines
The sample of step (6) after dry is placed in Muffle furnace and is calcined, to remove possible remaining organic matter, finally obtains single point
Scattered TiO2Microspheres product.
2. a kind of monodisperse TiO based on microemulsion according to claim 12The synthetic method of microballoon, it is characterised in that: micro-
Lotion is that partial hydrolysis and the polydisperse system that is formed are grasped through centrifugation in water by the acetylacetonate complex of tetra-n-butyl titanate
Make and is formed.
3. a kind of monodisperse TiO based on microemulsion according to claim 12The synthetic method of microballoon, it is characterised in that:
TiO2The size adjustment method of microballoon are as follows: diluted the upper layer transparent dispersion after step (3) centrifugation with deionized water, deionization
The research on maximum utilized quantity of water is 4 times that original volume is diluted to after deionized water is added, then through identical hydro-thermal, washing and back tender
Skill obtains product.
4. a kind of monodisperse TiO based on microemulsion according to claim 12The synthetic method of microballoon, it is characterised in that: step
Suddenly in (6) sample drying condition are as follows: dry 2h at a temperature of 100 DEG C.
5. a kind of monodisperse TiO based on microemulsion according to claim 12The synthetic method of microballoon, it is characterised in that: step
Suddenly the calcination condition in (7) are as follows: 550 DEG C of temperature lower calcination 1h.
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