CN1454939A - Method of preparing nano titanium dioxide granule with surface coated of aluminium oxide - Google Patents
Method of preparing nano titanium dioxide granule with surface coated of aluminium oxide Download PDFInfo
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- CN1454939A CN1454939A CN 03140530 CN03140530A CN1454939A CN 1454939 A CN1454939 A CN 1454939A CN 03140530 CN03140530 CN 03140530 CN 03140530 A CN03140530 A CN 03140530A CN 1454939 A CN1454939 A CN 1454939A
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Abstract
The preparation method of nano titanium dioxide granule whose surface is coated with aluminium oxide includes the following steps: adopting gel-sol method to synthesize nano titanium dioxide, then coating its surface with aluminium oxide. The grain diameter of the prepared nano titanium dioxide is 10-100 nm, its surface is coated with aluminium oxide membrane. Said nano titanium dioxide coated with aluminium dioxide has good dispersion property, can implement single granule dispersion, can be used as excellent UV-ray screening agent, and can be used in the fields of paint, rubber, fibre, coating material, sun protection products, printing ink and food package, etc.
Description
Affiliated field:
The invention belongs to a kind of synthetic method of inorganic nano material, relate to a kind of preparation method of titanium dioxide nanoparticle of surface-coating aluminum oxide specifically.
Background technology:
Nano titanium oxide primary particle diameter has lost the iris action to visible light between 10-100nm, become can absorb and " transparent titanium dioxide " of the UV-light that the scattering wavelength is shorter.Has excellent ultravioletlight screening, can shield long wave (380-320nm), medium wave (320-290nm) and shortwave (290-220nm) ultraviolet ray, has the superiority that the agent of organism ultravioletlight screening hardly matches, and have erosion resistance, a higher chemical stability, nontoxic, be widely used in fields such as high-quality coating, rubber, fiber, paint, sun-proof skin care articles for use, printing ink, food product pack as a kind of ultravioletlight screening agent of excellence.
But nano titanium oxide has strong photoxidation ability simultaneously, is a kind of photocatalyst material of excellence simultaneously, can degradation of organic substances, and therefore when being used for coating, makeup, to organic constituents generation photodegradation.Therefore need cover its surface light avtive spot to the nano titanium oxide surface treatment.Nano titanium oxide is reunited extremely easily simultaneously, usually adopt powerful the dispersion, also still have many aggregated particles to exist, nano titanium oxide disperses bad in base-material, its ultraviolet screener performance is not in full use, and it also is very necessary therefore improving its dispersiveness.Patent WO 90/06103 has reported that the dispersing nanometer titanium dioxide performance of phosphoric acid fat coating is improved, and has improved the ability of its shielding UV-light.US5,840,111 adopt the dispersive ability of the method raising titanium dioxide nanoparticle of surface-coating Cs2O and ferric oxide.US5,415,936 have adopted the hydrophobic ability of the method raising nano titanium oxide of surface organic modification.But separately with the alumina treatment nano titanium oxide to improve its dispersing property and weathering resistance, report not also.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of titanium dioxide nanoparticle of surface-coating aluminum oxide.
The present invention is at first to be raw material with the tetrabutyl titanate, adopts sol-gel method to prepare titanium dioxide nanoparticle, carries out the aluminum oxide coating then and handles.
Preparation method's concrete steps of the present invention are as follows:
1, with Ti (OC
4H
9)
4Be dissolved in the ethanol Ti (OC
4H
9)
4With the alcoholic acid volume ratio be 1: 5-15, the tetrabutyl titanate solution A; Water-soluble in ethanol, water and alcoholic acid volume ratio are 1: 1-10, the alcoholic solution B of water, sodium aluminate added be mixed with Al in the sodium hydroxide solution
2O
3Content is 0.1-5.0wt%, and NaOH content is the sodium aluminate alkali solution C of 0.2-7.5Wt%;
2, under the room temperature, in 10-120min, press Ti (OC
4H
9)
4With the mol ratio of water be 1: 50-200 adds solution A in the solution B of vigorous stirring slaking 10-60min, suction filtration, 100-150 ℃ of oven dry;
3, will dry powder and grind, 400-1000 ℃ of roasting gets anatase titanium dioxide or rutile type nano titanic oxide;
4, above-mentioned titanium dioxide is pressed TiO
2Quality is that 2-15% is scattered in the water than concentration, adds sodium hexametaphosphate dispersant, and its mass ratio is P
2O
5: TiO
2=0.1-0.5: 100, the pH value of regulating nano titanium dioxide paste liquid with NaOH solution is 8-10, ultra-sonic dispersion 0.5-1h;
5, with the dispersive nano-TiO
2Slurries are heated to 60-95 ℃, are adjusted to the pH value and are 8-10, form solution D, in 20-90min the solution D constant current are added solution C, and the pH value with sulfuric acid adjusting slurries remains on the former pH value of solution D simultaneously, and its add-on is Al by mass ratio
2O
3: TiO
2=1-20: 100;
6, reacted slurries stir slaking 30-180 minute;
7, it is neutral regulating the pH value with sulphuric acid soln then, stirs 30-100 minute;
8, filtration, secondary deionized water washing are to the no SO of check
4 2-, 100-150 ℃ of oven dry promptly gets monodispersed surface-coating aluminium oxide nano titanium dioxide granule.
The present invention compared with prior art has following advantage:
1. the inventive method is simple, and is easy to operate.
2. the product particle diameter that makes of the present invention is between 10-100nm, this nano titanium oxide surface-coating has aluminum oxide, and has a good dispersing property, can be used as excellent ultravioletlight screening agent, be used for fields such as coating, rubber, fiber, paint, sun-proof skin care articles for use, printing ink, food product pack.
Embodiment:
Embodiment 1
250g Ti (OC
4H
9)
4Be dissolved in the 2500ml ethanol, get Ti (OC
4H
9)
4Solution A; The ethanol of 1320ml is dissolved in the water of 1320ml, is solution B; Preparation sodium aluminate alkali solution C (mass percentage concentration: Al
2O
3%=0.28% NaOH%=0.45%), under the room temperature, pumped into solution A in 50 minutes in the solution B of vigorous stirring, continued to stir 15 minutes suction filtration, the xerogel of 110 ℃ of oven dry in following 15 hours.Grind above-mentioned xerogel, 80 order Microtraps sieve, and 500 ℃ of following roastings obtained nanometer anatase titania in 1 hour.Above-mentioned nano titanium oxide 10g is scattered in the water of 300ml, presses P
2O
5: TiO
2=0.1% adds sodium hexametaphosphate dispersant, and it is 10 that the NaOH of 1M regulates PH, ultra-sonic dispersion 50 minutes.With nano-TiO
2Slurries under agitation, are heated to 85 ℃, and regulating the pH value then is 8.5, adds solution C then in 40 minutes, with Al
2O
3The weight meter, Al
2O
3: TiO
2=10%, slaking 3 hours.The pH value of regulating slurries with sulphuric acid soln is 7.0, stirs then 30 minutes.Filtration, secondary deionized water washing washing are to the no SO of check
4 2-, 120 ℃ of oven dry in following 15 hours promptly get monodispersed surface-coating aluminium oxide nano titanium dioxide granule.
The titania nanoparticles diameter that electron microscope is observed this kind aluminum oxide coating down is 40-60nm.The XRD measuring result shows that titanium dioxide is anatase titanium dioxide.
Embodiment 2
Adopt the preparation process of the foregoing description 1, difference is that the dry gel powder roasting is that temperature is following 10 hours at 800 ℃, what obtain is rutile type nano titanic oxide, continue to adopt above-mentioned steps to carry out the aluminum oxide coating, obtain the rutile type nano titanic oxide of monodispersed aluminum oxide coating.It is 90-100nm that electron microscope is observed this kind nanometer anatase titanium dioxide particle diameter down.
Embodiment 3
25g Ti (OC
4H
9)
4Be dissolved in the 500ml ethanol, get solution A; The ethanol of 130ml is dissolved in the water of 370ml, is solution B; Preparation sodium aluminate alkali solution C (concentration: Al
2O
3%wt=0.28% NaOH%wt=0.45%), under the room temperature, pumped into solution A in 60 minutes in the solution B of vigorous stirring, continued to stir 15 minutes suction filtration, the xerogel of 100 ℃-130 ℃ oven dry in following 15 hours.Grind above-mentioned xerogel, 80 order Microtraps sieve, and 500 ℃ of following roastings got nanometer anatase titania in 1 hour.Above-mentioned nano titanium oxide 8g is scattered in the water of 300ml, presses P
2O
5: TiO
2=0.1%wt adds sodium hexametaphosphate dispersant, and it is 10 that the NaOH of 2.5M regulates PH, ultra-sonic dispersion 50 minutes.With nano-TiO
2Slurries under agitation, are heated to 85 ℃, and regulating the pH value then is 8.5, and constant current adds solution C in 45 minutes then, with Al
2O
3The weight meter, Al
2O
3: TiO
2=10%, slaking 3 hours.The pH value of regulating slurries with the sulphuric acid soln of 10%v/v is 7.0, stirs then 30 minutes.Filtration, secondary deionized water washing washing are to the no SO of check
4 2-, 120 ℃ of oven dry in following 15 hours promptly get monodispersed surface-coating aluminium oxide nano titanium dioxide granule.
It is 60-100nm that electron microscope is observed this kind nanometer anatase titanium dioxide particle diameter down.
Embodiment 4
250g Ti (OC
4H
9)
4Be dissolved in the 2500ml ethanol, get solution A; The ethanol of 1320ml is dissolved in the water of 1320ml, is solution B; Preparation sodium aluminate alkali solution C (mass percentage concentration: Al
2O
3%=5% NaOH%=7.5%), under the room temperature, pumped into solution A in 50 minutes in the solution B of vigorous stirring, continued to stir 15 minutes suction filtration, the xerogel of 110 ℃ of oven dry in following 15 hours.Grind above-mentioned xerogel, 80 order Microtraps sieve, and 500 ℃ of following roastings got nanometer anatase titania in 1 hour.Above-mentioned nano titanium oxide 10g is scattered in the water of 300ml, presses P
2O
5: TiO
2=0.1% adds sodium hexametaphosphate dispersant, and it is 10 that the NaOH of 2.5M regulates pH, ultra-sonic dispersion 50 minutes.With nano-TiO
2Slurries under agitation, are heated to 95 ℃, and regulating the pH value then is 8.5, adds solution C then in 60 minutes, with Al
2O
3The weight meter, Al
2O
3: TiO
2=15%, slaking 3 hours.The pH value of regulating slurries with the sulphuric acid soln of 10%v/v is 7.0, stirs then 30 minutes.Filtration, secondary deionized water washing washing are to the no SO of check
4 2-, 120 ℃ of oven dry in following 15 hours promptly obtain monodispersed surface-coating aluminium oxide nano titanium dioxide granule.
The titania nanoparticles diameter that electron microscope is observed this kind aluminum oxide coating down is 40-60nm.The XRD measuring result shows that titanium dioxide is anatase titanium dioxide.
Claims (1)
1. the preparation method of the titanium dioxide nanoparticle of a surface-coating aluminum oxide is characterized in that comprising the steps:
(1) with Ti (OC
4H
9)
4Be dissolved in the ethanol Ti (OC
4H
9)
4With the alcoholic acid volume ratio be 1: 5-15, the tetrabutyl titanate solution A; Water-soluble in ethanol, water and alcoholic acid volume ratio are 1: 1-10, the alcoholic solution B of water, sodium aluminate added be mixed with Al in the sodium hydroxide solution
2O
3Content is 0.1-5.0wt%, and NaOH content is the sodium aluminate alkali solution C of 0.2-7.5Wt%;
(2) under the room temperature, in 10-120min, press Ti (OC
4H
9)
4With the mol ratio of water be 1: 50-200 adds solution A in the solution B of vigorous stirring slaking 10-60min, suction filtration, 100-150 ℃ of oven dry;
(3) will dry powder and grind, 400-1000 ℃ of roasting gets anatase titanium dioxide or rutile type nano titanic oxide;
(4) above-mentioned titanium dioxide is pressed TiO
2Quality is that 2-15% is scattered in the water than concentration, adds sodium hexametaphosphate dispersant, and its mass ratio is P
2O
5: TiO
2=0.1-0.5: 100, the pH value of regulating nano titanium dioxide paste liquid with NaOH solution is 8-10, ultra-sonic dispersion 0.5-1h;
(5) with the dispersive nano-TiO
2Slurries are heated to 60-95 ℃, are adjusted to the pH value and are 8-10, form solution D, in 20-90min the solution D constant current are added solution C, and the pH value with sulfuric acid adjusting slurries remains on the former pH value of solution D simultaneously, and its add-on is Al by mass ratio
2O
3: TiO
2=1-20: 100;
(6) reacted slurries stir slaking 30-180 minute;
(7) it is neutral regulating the pH value with sulphuric acid soln then, stirs 30-100 minute;
(8) filtration, secondary deionized water washing are to the no SO of check
4 2-, 100-150 ℃ of oven dry promptly gets monodispersed surface-coating aluminium oxide nano titanium dioxide granule.
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| CN100528976C (en) * | 2006-12-20 | 2009-08-19 | 中国科学院山西煤炭化学研究所 | Method for coating surface of white titanium pigment |
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| CN101367548B (en) * | 2008-09-12 | 2011-06-29 | 江苏工业学院 | Method of preparing hydrophobic nano-titanium dioxide powder |
| CN101255288B (en) * | 2007-11-29 | 2011-09-21 | 江苏河海纳米科技股份有限公司 | Nano titanium oxide inorganic surface treatment method |
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