CN105502486A - Method for preparing rice-shaped rutile-phase titanium dioxide nano particles - Google Patents
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Abstract
The invention discloses a method for preparing rice-shaped rutile-phase titanium dioxide nano particles. The method comprises the following steps that 1, 12 g to 16 g of P123 is dissolved into 460 ml to 480 ml of 0.43 mol/L hydrochloric acid, and stirring is carried out to obtain a clear P123-hydrochloric acid solution; 2, 51 g to 53 g of tetrabutyl titanate is added to the P123-hydrochloric acid solution prepared in the step 1, and stirring is carried out for hydrolysis for 60-72 hours at the temperature of 35 DEG C; 3, hydrolyzed turbid liquid obtained after hydrolysis of the step 2 is centrifuged, and white solids are separated out, and washed with deionized water; 4, the white solids obtained in the step 3 are dried at room temperature, and the rice-shaped rutile-phase titanium dioxide nano particles are obtained. The rutile-phase titanium dioxide nano particles prepared through the method are high in purity, and the preparation steps are relatively simple.
Description
Technical field
The present invention relates to and belong to by wet production, as the preparation method of hydrolysising titanium salt, be specifically related to a kind of preparation method of grain of rice shape red schorl phase titanium dioxide nano particle.
Background technology
Titanic oxide material mainly has three kinds of crystalline phases, Detitanium-ore-type (Anatase), rutile-type (Rutile) and brookite type (Brookite).Wherein, Detitanium-ore-type and rutile-type are widely used.Rutile is the crystalline phase of thermodynamic stable, and anatase octahedrite is the crystalline phase of dynamic stabilization, and in high-temperature calcination process, anatase octahedrite can change to rutile, according to its transformation temperature of difference of titanic oxide material character from 400 DEG C to 1200 DEG C not etc.Under normal circumstances, the temperature that pure anatase titanium dioxide is converted into rutile-type is 610 DEG C-915 DEG C, and as anatase titanium dioxide will be made to be converted into rutile-type completely, then calcining temperature should higher than 1000 DEG C.
That has reported at present prepares in the method for titanic oxide material, if otherwise the process through high-temperature roasting obtains pure red schorl phase titanium dioxide, and mainly use titanium tetrachloride or titanium tetrafluoride to be hydrolyzed preparation for raw material.If use common tetrabutyl titanate to be hydrolyzed for raw material, generally can only obtain the titanium dioxide of Anatase, then just can obtain red schorl phase titanium dioxide through high-temperature roasting.Adopt tetrabutyl titanate hydrolysis, then obtain through high-temperature calcination process the high-temperature calcination process that red schorl phase titanium dioxide material not only needs through high energy consumption, and assemble-sintering because high-temperature roasting can cause TiO 2 particles, be difficult to obtain titanium dioxide nano-particle.
Also the document preparing red schorl phase titanium dioxide nano particle under having low temperature is at present open, if patent publication No. is that a kind of of CN103833074A prepares in the method for titanium dioxide nano-particle, tetrabutyl titanate, concentrated hydrochloric acid are joined in the mixed solvent of hexanaphthene and ethanol, under the condition of backflow, is obtained by reacting monodispersed anatase phase titanium dioxide nanoparticle.By strengthening the consumption of concentrated hydrochloric acid, product can be made to be changed to Rutile Type gradually by Anatase, and can finally obtain pure phase Rutile Type.The anatase phase titanium dioxide nanoparticle obtained is single dispersing, and particle diameter is less than 5nm; The particle diameter of the red schorl phase titanium dioxide nano particle obtained is less than 10nm.Generally have Anatase, red schorl phase titanium dioxide nano mix particles in above-mentioned preparation method, what be difficult to guarantee preparation is exactly red schorl phase titanium dioxide nano particle.
In addition, patent publication No. is in a kind of method of low-temperature growth nanometer rutile phase titanic oxide of CN1351962A, first tetrabutyl titanate and ethanol are made into reaction soln A, deionized water and nitric acid are made into reaction soln B, then solution A is slowly added in solution B, this solution stirring is become homogeneous solution, at room temperature continuation stirring makes it complete hydrolysis again becomes colloidal sol, finally colloidal sol is incubated 5 ~ 20 hours in 30 ~ 60 DEG C, colloidal sol gradually becomes gel, become powder, namely obtain nanometer rutile phase titanic oxide.Aforesaid method is added by tetrabutyl titanate first to form colloidal sol (sol) afterwards, then form gel (gel), is actually sol-gel method and is prepared, and above-mentioned preparation process relative complex.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of grain of rice shape red schorl phase titanium dioxide nano particle, the red schorl phase titanium dioxide nano particle purity that this preparation method prepares gained is high, and preparation process is relatively simple.
For achieving the above object, base case of the present invention is as follows:
A preparation method for grain of rice shape red schorl phase titanium dioxide nano particle, comprises the following steps:
(1) be dissolved in the hydrochloric acid of 460-480ml by 14-16gP123, stir the P123-hydrochloric acid soln obtaining clarifying, the concentration of described hydrochloric acid is 0.4-0.45mol/L;
(2) 51-53g tetrabutyl titanate is added in P123-hydrochloric acid soln prepared by step 1, at the temperature of 32-35 DEG C, stir hydrolysis 60-75 hour;
(3) the hydrolysis suspension liquid obtained after step 2 being hydrolyzed is centrifugal, isolates white solid, and with deionized water rinsing;
(4) white solid step 3 obtained is at room temperature dry, namely obtains grain of rice shape Rutile Type dioxy
Change titanium nanoparticle.
The effect of this programme: 1, use common tetrabutyl titanate for titanium source, be hydrolyzed at the temperature of 32-35 DEG C in the hydrochloric acid soln of P123, hydrolysate at room temperature seasoning after centrifugation, washing directly can obtain the red schorl phase titanium dioxide material of single crystalline phase, and purity is high, substantially can more than 99.9% be reached; 2, the red schorl phase titanium dioxide material adopting preparation method of the present invention to obtain is the nanoparticle of very uniform grain of rice shape, size is at about 80nm × 10nm, above-mentioned uniform nanoparticle does not need stage treatment in use, compared with the nanoparticle that size is mixed and disorderly, use value is higher, such as, when the uniform nanoparticle of above-mentioned size is as catalyzer, can ensure that the avtive spot of every particle is even, thus ensureing that the catalytic performance of every nanoparticle is even, using value is very high in the field of study; When and for example the uniform nanoparticle of above-mentioned size is as support of the catalyst, can make catalyzed material diffusion evenly, resistance to mass transfer is even, thus improves catalytic effect; 3, the hydrolysis temperature in this programme preparation process is at about 30 DEG C, and preparation process does not need the hydrothermal treatment process of high-temperature calcination process through any high energy consumption or complexity, and preparation process is relatively simple, and saves the energy.
Prioritization scheme 1, to the further optimization of base case, the quality of described P123 is 15.5g; Hydrochloric acid volume is 480ml, and concentration is 0.43mol/L; The quality of tetrabutyl titanate is 52.54g.Contriver finds through experiment, and the purity of the red schorl phase titanium dioxide material adopting the raw material of said ratio to prepare is higher, and the size uniform of nanoparticle.
Prioritization scheme 2, to the further optimization of base case, after step 1, by the stirred in water bath 25-35 minute of P123-hydrochloric acid soln at 35 DEG C, stirring frequency is 150-200r/min.P123-hydrochloric acid soln in a water bath heating energy ensures homogeneous heating, and the stirring frequency of above-mentioned scope can make P123-hydrochloric acid soln more even, thus make subsequent reactions process faster, and experiment finds after above-mentioned process, purity and the homogeneity of the nanoparticle prepared increase.
Prioritization scheme 3, to the further optimization of base case, any one of prioritization scheme 1,2, in step 2, adding of described tetrabutyl titanate adopts glue head dropper 30-40 to drip/min dropping, employing aforesaid way tetrabutyl titanate is added P123-hydrochloric acid soln, can particle be made evenly.
Prioritization scheme 4, to the further optimization of base case, any one of prioritization scheme 1,2, stirs hydrolysis 72 hours in a water bath in step 2.After the stirred in water bath hydrolysis above-mentioned time, fully can react between raw material, generate more red schorl phase titanium dioxide nano particle.
Accompanying drawing explanation
The scanning electron microscope (SEM) photograph of the titanium dioxide nano-particle prepared by Fig. 1 embodiment of the present invention 1;
The transmission electron microscope picture of the titanium dioxide nano-particle prepared by Fig. 2 embodiment of the present invention 1;
The XRD spectra of the titanium dioxide nano-particle prepared by Fig. 3 embodiment of the present invention 1;
The uv raman spectroscopy figure of the titanium dioxide nano-particle prepared by Fig. 4 embodiment of the present invention 1;
The visible Raman spectrogram of the titanium dioxide nano-particle prepared by Fig. 5 embodiment of the present invention 1.
Embodiment
Below by embodiment, the present invention is further detailed explanation:
In following embodiment, mentioned P123 is a kind of triblock copolymer, and full name is: polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer, is a kind of nonionogenic tenside.
Only illustrate for embodiment 1 method preparing grain of rice shape red schorl phase titanium dioxide nano particle below, other embodiments only list the difference part with embodiment 1, and all embodiments represent all in Table 1.
Embodiment 1
A preparation method for grain of rice shape red schorl phase titanium dioxide nano particle, comprises the following steps:
(1) be dissolved in the hydrochloric acid of 480ml by 15.5gP123, stir the P123-hydrochloric acid soln obtaining clarifying, the concentration of described hydrochloric acid is 0.43mol/L;
(2) 52.54g tetrabutyl titanate glue head dropper is added dropwise in the P123-hydrochloric acid soln of step 1 preparation with 35/min, under the bath temperature of 35 DEG C, stirs hydrolysis 72 hours;
(3) the hydrolysis suspension liquid obtained after step 2 being hydrolyzed is centrifugal in centrifuges, isolates white solid, and with deionized water rinsing;
(4) white solid step 3 obtained is at room temperature dry, namely obtains grain of rice shape red schorl phase titanium dioxide nano particle.
Embodiment 4
The difference part of the present embodiment and embodiment 1 is, after step 1, by the stirred in water bath 30 minute of P123-hydrochloric acid soln at 35 DEG C, stirring frequency is 150-200r/min.P123-hydrochloric acid soln in a water bath heating energy ensures homogeneous heating, thus makes subsequent reactions process faster, and experiment finds after above-mentioned process, and purity and the homogeneity of the nanoparticle prepared increase.
Table 1
The rutile-phase nano particle for preparing of Example 1-5 below, detect its purity and particle uniformity respectively, wherein homogeneity represents with the quantity of *, and * quantity is more, and represent that nanoparticle is more even, result is as table 2:
Table 2
As can be drawn from Table 2 to draw a conclusion:
1, embodiment 1 is compared with embodiment 4, and difference is embodiment 4 after step 1, by P123-hydrochloric acid soln moderate-speed mixer 30 minutes in the water-bath of 35 DEG C.Thus can find out, through above-mentioned treatment step, the nanoparticle purity and particle uniformity that prepare can be improved;
The purity of the red schorl phase titanium dioxide nano particle 2, prepared in embodiment 1-5 is all more than 99%, and purity is very high.
Can draw to draw a conclusion by the detected result accompanying drawing 1-5 observing the red schorl phase titanium dioxide nano particle that embodiment 1 prepares:
1, Fig. 1 is the scanning electron microscope (SEM) photograph of the titanium dioxide nano-particle material prepared by the embodiment of the present invention 1.Fig. 2 is the transmission electron microscope picture of the titanium dioxide nano-particle material prepared by the embodiment of the present invention 1.Composition graphs 1 and Fig. 2 can find out that the titanium dioxide nano-particle material prepared by the present invention has the pattern of grain of rice shape, and size is at about 80nm × 10nm.
The XRD spectra of the titanium dioxide nano-particle material 2, gone out synthesized by Fig. 3 embodiment of the present invention 1.Can find out that the titanium dioxide nano-particle material prepared by the present invention has the diffraction peak consistent with red schorl phase titanium dioxide standard substance, this illustrates that its crystalline phase is Rutile Type.In addition, can see that the width that the width that the XRD of the titanium dioxide nano-particle material prepared by the present invention composes peak obviously composes peak than the XRD of two kinds of titanium dioxide standard substance is large, this also illustrates that its size of particles is significantly less than the size of particles of two kinds of titanium dioxide standard substance, and the Electronic Speculum test result of Fig. 1, Fig. 2 matches.
3, Fig. 4 is uv raman spectroscopy figure and the visible Raman spectrogram of titanium dioxide nano-particle material prepared by the embodiment of the present invention 1.The excitation wavelength of visible Raman spectrum test is 532nm, and the excitation wavelength of uv raman spectroscopy test is 325nm, and the spectrum peak in these two kinds of Raman spectrograms is all the spectrum peak of typical red schorl phase titanium dioxide.Because visible Raman spectrum test is the information of the inside nanoparticles of reflection more, two uv raman spectroscopy tests are the information of the nanoparticle surface of reflection more, so the ultraviolet Raman of composition graphs 4 and visible Raman spectrogram, no matter the titanium dioxide nano-particle that we can know prepared by the embodiment of the present invention 1 is inside particles or particle surface is all rutile phase.
Above-described is only embodiments of the invention, and in scheme, the general knowledge such as known characteristic does not do too much description at this.Should be understood that; for a person skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made; these also should be considered as protection scope of the present invention, and these all can not affect effect of the invention process and practical applicability.The protection domain that this application claims should be as the criterion with the content of its claim, and the embodiment in specification sheets etc. record the content that may be used for explaining claim.
Claims (5)
1. a preparation method for grain of rice shape red schorl phase titanium dioxide nano particle, is characterized in that, comprise the following steps:
(1) be dissolved in the hydrochloric acid of 460-480ml by 14-16gP123, stir the P123-hydrochloric acid soln obtaining clarifying, the concentration of described hydrochloric acid is 0.4-0.45mol/L;
(2) 51-53g tetrabutyl titanate is added in P123-hydrochloric acid soln prepared by step 1, at the temperature of 32-35 DEG C, stir hydrolysis 60-75 hour;
(3) the hydrolysis suspension liquid obtained after step 2 being hydrolyzed is centrifugal, isolates white solid, and with deionized water rinsing;
(4) white solid step 3 obtained is at room temperature dry, namely obtains grain of rice shape red schorl phase titanium dioxide nano particle.
2. the preparation method of a kind of grain of rice shape red schorl phase titanium dioxide nano particle according to claim 1, it is characterized in that, the quality of described P123 is 15.5g; Hydrochloric acid volume is 480ml, and concentration is 0.43mol/L; The quality of tetrabutyl titanate is 52.54g.
3. the preparation method of a kind of grain of rice shape red schorl phase titanium dioxide nano particle according to claim 1, it is characterized in that, after step 1, by the stirred in water bath 25-35 minute of P123-hydrochloric acid soln at 35 DEG C, stirring frequency is 150-200r/min.
4. the preparation method of a kind of grain of rice shape red schorl phase titanium dioxide nano particle according to any one of claim 1-3, is characterized in that, in step 2, adding of described tetrabutyl titanate adopts glue head dropper 30-40 to drip/min dropping.
5. the preparation method of a kind of grain of rice shape red schorl phase titanium dioxide nano particle according to any one of claim 1-3, is characterized in that, stir hydrolysis in a water bath 72 hours in step 2.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106935843A (en) * | 2017-03-23 | 2017-07-07 | 复旦大学 | A kind of rutile-phase nano-titanium dioxide and its low temperature preparation method and application |
| CN111607210A (en) * | 2020-05-28 | 2020-09-01 | 宁波德伟电器有限公司 | PC flame-retardant composite material for household appliances and preparation method thereof |
| CN111747445A (en) * | 2020-07-31 | 2020-10-09 | 重庆工商大学 | TiO 22-SiO2Oxide composite material and preparation method thereof |
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| CN1594101A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
| CN1821085A (en) * | 2006-03-03 | 2006-08-23 | 厦门大学 | Process for preparing nano mesoporous titanium dioxide at low tempeature |
| EP2724985A1 (en) * | 2012-10-24 | 2014-04-30 | Titan Kogyo Kabushiki Kaisha | Rutile-type titanium dioxide and cosmetics using the same |
| CN104016405A (en) * | 2014-05-30 | 2014-09-03 | 武汉理工大学 | Flower-shaped mesoporous titanium dioxide material and preparation method and application thereof |
| CN104828862A (en) * | 2015-04-03 | 2015-08-12 | 西南民族大学 | Preparation method of water-soluble anatase titanium dioxide nanopowder |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1594101A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
| CN1821085A (en) * | 2006-03-03 | 2006-08-23 | 厦门大学 | Process for preparing nano mesoporous titanium dioxide at low tempeature |
| EP2724985A1 (en) * | 2012-10-24 | 2014-04-30 | Titan Kogyo Kabushiki Kaisha | Rutile-type titanium dioxide and cosmetics using the same |
| CN104016405A (en) * | 2014-05-30 | 2014-09-03 | 武汉理工大学 | Flower-shaped mesoporous titanium dioxide material and preparation method and application thereof |
| CN104828862A (en) * | 2015-04-03 | 2015-08-12 | 西南民族大学 | Preparation method of water-soluble anatase titanium dioxide nanopowder |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106935843A (en) * | 2017-03-23 | 2017-07-07 | 复旦大学 | A kind of rutile-phase nano-titanium dioxide and its low temperature preparation method and application |
| CN111607210A (en) * | 2020-05-28 | 2020-09-01 | 宁波德伟电器有限公司 | PC flame-retardant composite material for household appliances and preparation method thereof |
| CN111747445A (en) * | 2020-07-31 | 2020-10-09 | 重庆工商大学 | TiO 22-SiO2Oxide composite material and preparation method thereof |
| CN111747445B (en) * | 2020-07-31 | 2022-09-09 | 重庆工商大学 | TiO 2 2 -SiO 2 Oxide composite material and preparation method thereof |
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