CN101062782A - Method for synthesizing nano titanium oxide colloid particle - Google Patents
Method for synthesizing nano titanium oxide colloid particle Download PDFInfo
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- CN101062782A CN101062782A CN 200610124301 CN200610124301A CN101062782A CN 101062782 A CN101062782 A CN 101062782A CN 200610124301 CN200610124301 CN 200610124301 CN 200610124301 A CN200610124301 A CN 200610124301A CN 101062782 A CN101062782 A CN 101062782A
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- Prior art keywords
- titanium oxide
- oxide colloid
- nano titanium
- colloid particle
- tetrabutyl titanate
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000002245 particle Substances 0.000 title claims abstract description 33
- 239000000084 colloidal system Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title abstract description 12
- 230000002194 synthesizing effect Effects 0.000 title 1
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 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 description 19
- 238000010189 synthetic method Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000012467 final product Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 abstract 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 abstract 2
- 235000013772 propylene glycol Nutrition 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 235000010215 titanium dioxide Nutrition 0.000 description 6
- 239000004408 titanium dioxide Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- -1 papermaking Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
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Abstract
The invention discloses a synthesized method of nanometer titanium oxide colloid particle, which comprises the following steps: dropping butyl titanate into 1,2-dihydroxypropane or 1,4-butanediol; setting molar concentration of butyl titanate at 0. 5-1. 0mol/L in the mixing solution; stirring; mixing evenly; proceeding hydrothermal reaction for 4. 0-48 h at 180-220 deg. c; getting the product. This invention possesses friendship environment, low temperature and does not need calcinations, which product does not need further surface treatment.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, be specifically related to a kind of synthetic method of nano titanium oxide colloid particle.
Background technology
Titanium dioxide is commonly called as titanium white, it is a kind of white inorganic pigment, have nontoxic, best opacity, best whiteness and luminance brightness, be considered to the present best a kind of white pigment of performance in the world, be widely used in industry such as coating, plastics, papermaking, ink printing, chemical fibre, rubber, pottery, makeup and medicine.Nano titanium oxide has very strong absorption ultraviolet ray ability, peculiar colour effect, the characteristic of thermostability, chemical stability and good aspects such as optics, electricity and mechanics preferably, has extensively and the potential application prospect in fields such as support of the catalyst, UV light absorber, efficient light-sensitive catalyst, sun-proof skin care shape product, plastic membrane product, water treatment, fine ceramics, ecological ceramic and gas sensor elements.
The preparation method of nano-titanium dioxide powder is more at present, mainly contains sol-gel method, hydrothermal method, hydrolysis method, the precipitator method, vapour deposition process etc.Vapor phase process can make that crystalline structure is good, purity is high, the uniform nano titanium oxide of size distribution, and good reproducibility; But vapor phase process generally needs pyroreaction, and this has just determined that also it is higher to equipment requirements, invests greatlyyer, and operational condition is harsh.The liquid phase method reaction conditions realizes that more easily therefore many now employing liquid phase methods prepare nano titanium oxide.But except hydrothermal method, general liquid phase method is the presoma of preparation titanium dioxide earlier, again with presoma calcining preparation titanium dioxide powder, be that reaction needed is through high-temperature calcination, this not only consumes a large amount of energy, and products obtained therefrom easily reunites, and size distribution is inhomogeneous.Hydro-thermal reaction is to carry out under non-confined condition, compares with other wet chemical method to have environmental friendliness, low temperature, need not calcine and can directly in solution, obtain product, and the product purity height, good dispersity does not have and reunites, etc. advantage.But current hydro-thermal reaction mainly is to be used to prepare nano-titanium dioxide powder, and utilizes the method for hydro-thermal reaction synthesis of nano titanium oxide colloid particle not appear in the newspapers as yet.
In use can there be agglomeration in nano-titanium dioxide powder, thereby makes nano titanium oxide can not give full play to the nano material effect because its particle size is less.Generally in use all adding a large amount of tensio-active agents carries out surface modification to it, and it is dispersed preferably that it is had, yet increased production cost like this in industry undoubtedly.
Summary of the invention
Main purpose of the present invention is to overcome the shortcoming of prior art, and a kind of synthetic method of nano titanium oxide colloid particle is provided, and gained titanium dioxide is Detitanium-ore-type, and its particle size is less than 10nm, and its particle size can be controlled by reaction conditions.
Purpose of the present invention is achieved through the following technical solutions:
A kind of synthetic method of nano titanium oxide colloid particle: tetrabutyl titanate is slowly splashed into 1,2-propylene glycol or 1, in the 4-butyleneglycol, the volumetric molar concentration of tetrabutyl titanate in mixed solution is 0.5～1.0mol/L, be stirred to and mix, in temperature is hydro-thermal reaction 4.0～48h under 180～220 ℃ of conditions, get final product nano titanium oxide colloid particle.
For further realizing purpose of the present invention, described hydro-thermal reaction is to carry out in having the teflon-lined autoclave.
Preferred 200～220 ℃ of the temperature of described hydro-thermal reaction.
The volumetric molar concentration of described tetrabutyl titanate in mixed solution is preferably 0.6～0.9mol/L.
With respect to prior art, the present invention has following advantage and beneficial effect:
(1) the present invention adopts hydrothermal method synthesis of nano titanium oxide colloid particle, compares with other wet chemical method to have environmental friendliness, low temperature, need not calcine advantages such as can directly obtaining product in solution.
(2) gained titanium oxide colloid particle of the present invention is the anatase-type nanometer titanium dioxide colloidal solid, and particle size is less than 10nm, and size is even, and good dispersity need not further surface treatment during use.
Description of drawings
Fig. 1 is the XRD figure of the prepared nano titanium oxide of experimental example of the present invention 1～6.
Fig. 2 is the transmission electron microscope photo of the prepared nano titanium oxide of the embodiment of the invention 3.
Embodiment
For better understanding the present invention, below in conjunction with embodiment the present invention is done detailed description further, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Embodiment 1
Tetrabutyl titanate is slowly splashed into 1, in the 2-propylene glycol, be stirred to and mix, the volumetric molar concentration of tetrabutyl titanate in mixing solutions is 0.5mol/L, change over to then and have in the teflon-lined autoclave, 220 ℃ of reaction 4h down make titanium oxide colloid particle in the thermostat container.Shown in curve among Fig. 11, all diffraction peaks can both be corresponding with the base peak of the Detitanium-ore-type of bottom, and hence one can see that, and the gained titanium oxide colloid particle is pure Detitanium-ore-type structure, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 4nm.
Tetrabutyl titanate is slowly splashed into 1, and in the 4-butyleneglycol, volumetric molar concentration and the operation of tetrabutyl titanate in mixing solutions is identical with enforcement 1, makes titanium oxide colloid particle.Shown in curve among Fig. 12, all diffraction peaks can both be corresponding with the base peak of the Detitanium-ore-type of bottom, and hence one can see that, and the gained titanium oxide colloid particle is pure Detitanium-ore-type structure, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 6nm.
Tetrabutyl titanate is slowly splashed into 1, in the 2-propylene glycol, be stirred to and mix, the volumetric molar concentration of tetrabutyl titanate in mixing solutions is 0.7mol/L, change over to then and have in the teflon-lined autoclave, 200 ℃ of reaction 24h down make titanium oxide colloid particle in the thermostat container.Shown in curve among Fig. 13, all diffraction peaks can both be corresponding with the base peak of the Detitanium-ore-type of bottom, and hence one can see that, and the gained titanium oxide colloid particle is pure Detitanium-ore-type structure, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 5nm.Fig. 2 is the transmission electron microscope photo of the nano titanium oxide of preparation.As shown in the figure, it is more even to further specify present embodiment gained titanium oxide colloid particle, and narrow diameter distribution is substantially all about 5nm, better dispersed.
Tetrabutyl titanate is slowly splashed into 1, and in the 4-butyleneglycol, volumetric molar concentration and the operation of tetrabutyl titanate in mixing solutions is identical with enforcement 1, makes titanium oxide colloid particle.Shown in curve among Fig. 14, all diffraction peaks can both be corresponding with the base peak of the Detitanium-ore-type of bottom, and hence one can see that, and the gained titanium oxide colloid particle is pure Detitanium-ore-type structure, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 8nm.
Tetrabutyl titanate is slowly splashed into 1, in the 2-propylene glycol, be stirred to and mix, the volumetric molar concentration of tetrabutyl titanate in mixing solutions is 1.0mol/L, change over to then and have in the teflon-lined autoclave, 180 ℃ of reaction 48h down make titanium oxide colloid particle in the thermostat container.Shown in curve among Fig. 15, all diffraction peaks can both be corresponding with the base peak of the Detitanium-ore-type of bottom, and hence one can see that, and the gained titanium oxide colloid particle is pure Detitanium-ore-type structure, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 8nm.
Tetrabutyl titanate is slowly splashed into 1, and in the 4-butyleneglycol, volumetric molar concentration and the operation of tetrabutyl titanate in mixing solutions is identical with enforcement 1, makes titanium oxide colloid particle.Shown in curve among Fig. 16, all diffraction peaks can both be corresponding with the base peak of the Detitanium-ore-type of bottom, hence one can see that, and the gained titanium oxide colloid particle is pure Detitanium-ore-type structure, by the halfwidth of broadening, can estimate that with the Scherrer formula grain-size is about 10nm.
Claims (5)
1, a kind of synthetic method of nano titanium oxide colloid particle, it is characterized in that: tetrabutyl titanate is slowly splashed into 1,2-propylene glycol or 1, in the 4-butyleneglycol, the volumetric molar concentration of tetrabutyl titanate in mixed solution is 0.5～1.0mol/L, being stirred to and mixing, is hydro-thermal reaction 4.0～48h under 180～220 ℃ of conditions in temperature, get final product nano titanium oxide colloid particle.
2, the synthetic method of nano titanium oxide colloid particle according to claim 1 is characterized in that, described hydro-thermal reaction is to carry out in having the teflon-lined autoclave.
According to the synthetic method of claim 1 or 2 described described nano titanium oxide colloid particles, it is characterized in that 3, the temperature of described hydro-thermal reaction is 200～220 ℃.
According to the synthetic method of claim 1 or 2 described described nano titanium oxide colloid particles, it is characterized in that 4, the volumetric molar concentration of tetrabutyl titanate in mixed solution is 0.6～0.9mol/L.
According to the synthetic method of the described described nano titanium oxide colloid particle of claim 3, it is characterized in that 5, the volumetric molar concentration of tetrabutyl titanate in mixed solution is 0.6～0.9mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101243010A CN100528757C (en) | 2006-12-19 | 2006-12-19 | Method for synthesizing nano titanium oxide colloid particle |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101243010A CN100528757C (en) | 2006-12-19 | 2006-12-19 | Method for synthesizing nano titanium oxide colloid particle |
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| CN101062782A true CN101062782A (en) | 2007-10-31 |
| CN100528757C CN100528757C (en) | 2009-08-19 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086047A (en) * | 2011-01-12 | 2011-06-08 | 宣城晶瑞新材料有限公司 | Titanium dioxide powder with ultrahigh water dispersion and high photocatalytic activity and preparation method thereof |
| CN105771824A (en) * | 2016-03-22 | 2016-07-20 | 陕西师范大学 | Method for preparing biomimetic microcapsule by confinement of organic titanium source and natural pigments in phospholipid bilayer |
| CN109501018A (en) * | 2018-09-19 | 2019-03-22 | 宣城福美达新材料有限公司 | A kind of high-intensity wood plastic composite |
| CN111204798A (en) * | 2020-03-05 | 2020-05-29 | 福州大学 | High-sensitivity two-dimensional nano strontium titanate gas-sensitive material with low working temperature and preparation method and application thereof |
-
2006
- 2006-12-19 CN CNB2006101243010A patent/CN100528757C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086047A (en) * | 2011-01-12 | 2011-06-08 | 宣城晶瑞新材料有限公司 | Titanium dioxide powder with ultrahigh water dispersion and high photocatalytic activity and preparation method thereof |
| CN102086047B (en) * | 2011-01-12 | 2012-05-30 | 宣城晶瑞新材料有限公司 | Titanium dioxide powder with ultrahigh water dispersion and high photocatalytic activity and preparation method thereof |
| CN105771824A (en) * | 2016-03-22 | 2016-07-20 | 陕西师范大学 | Method for preparing biomimetic microcapsule by confinement of organic titanium source and natural pigments in phospholipid bilayer |
| CN105771824B (en) * | 2016-03-22 | 2018-12-04 | 陕西师范大学 | A kind of method that phospholipid bilayer confinement organic titanium source, natural pigment prepare bionical micro-capsule |
| CN109501018A (en) * | 2018-09-19 | 2019-03-22 | 宣城福美达新材料有限公司 | A kind of high-intensity wood plastic composite |
| CN111204798A (en) * | 2020-03-05 | 2020-05-29 | 福州大学 | High-sensitivity two-dimensional nano strontium titanate gas-sensitive material with low working temperature and preparation method and application thereof |
| CN111204798B (en) * | 2020-03-05 | 2022-03-25 | 福州大学 | High-sensitivity two-dimensional nano strontium titanate gas-sensitive material with low working temperature and preparation method and application thereof |
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| Publication number | Publication date |
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| CN100528757C (en) | 2009-08-19 |
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Granted publication date: 20090819 Termination date: 20131219 |