CN105502486B - Method for preparing rice-shaped rutile-phase titanium dioxide nano particles - Google Patents
Method for preparing rice-shaped rutile-phase titanium dioxide nano particles Download PDFInfo
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- CN105502486B CN105502486B CN201510956002.2A CN201510956002A CN105502486B CN 105502486 B CN105502486 B CN 105502486B CN 201510956002 A CN201510956002 A CN 201510956002A CN 105502486 B CN105502486 B CN 105502486B
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- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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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
Wet production is used the present invention relates to belong to, such as the preparation method of hydrolysising titanium salt, and in particular to a kind of rice-shaped golden red
The preparation method of stone 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 plate titanium
Ore deposit type (Brookite).Wherein, Detitanium-ore-type and rutile-type are widely used.Rutile is the crystalline phase of thermodynamic stable, sharp
Titanium ore is the crystalline phase of dynamic stabilization, and anatase can change to rutile in high-temperature calcination process, according to titanic oxide material
Different its phase transition temperature of property are from 400 DEG C to 1200 DEG C.Under normal circumstances, pure anatase titanium dioxide is converted into gold
The temperature of red stone-type is 610 DEG C -915 DEG C, anatase titanium dioxide is fully converted to rutile-type, then calcining heat should be higher than
1000℃。
In the method for preparing titanic oxide material reported at present, if otherwise obtaining pure by the process of high-temperature roasting
Red schorl phase titanium dioxide, mainly using titanium tetrachloride or titanium tetrafluoride for raw material is hydrolyzed preparation.If used
Common butyl titanate is hydrolyzed for raw material, typically can only obtain the titanium dioxide of Anatase, is then roasted by high temperature
Burning can just obtain red schorl phase titanium dioxide.Using tetrabutyl titanate hydrolysis, then rutile is obtained by high-temperature calcination process
Phase titanium dioxide material is not only needed by the high-temperature calcination process of high energy consumption, and because high-temperature roasting can cause titanium dioxide
Particle buildup-sintering, hardly results in titanium dioxide nano-particle.
Also there is the document that red schorl phase titanium dioxide nano particle is prepared under low temperature to disclose at present, such as patent publication No. is
In a kind of method for preparing titanium dioxide nano-particle of CN103833074A, butyl titanate, concentrated hydrochloric acid are added to hexamethylene
In the mixed solvent of alkane and ethanol, reaction obtains monodispersed anatase phase titanium dioxide nano-particle under conditions of backflow.
By increasing the consumption of concentrated hydrochloric acid, product can be made gradually to be changed to Rutile Type from Anatase, and can finally obtain pure phase
Rutile Type.The anatase phase titanium dioxide nano-particle of acquisition is in single dispersing, and particle diameter is less than 5nm；The Rutile Type two of acquisition
The particle diameter of titanium oxide nanoparticles is less than 10nm.Typically Anatase, red schorl phase titanium dioxide are had in above-mentioned preparation method
Nano-particle mixes, it is difficult to which ensure preparation is exactly red schorl phase titanium dioxide nano particle.
In addition, method of the patent publication No. for a kind of low temperature preparation nanometer rutile phase titanic oxide of CN1351962A
In, butyl titanate and ethanol are made into reaction solution A first, deionized water and nitric acid are made into reaction solution B, then will be molten
Liquid A is slowly added in solution B, by the solution stirring turn into homogeneous solution, then at room temperature continue stirring be allowed to complete hydrolysis into
It is colloidal sol, colloidal sol is finally incubated 5~20 hours in 30~60 DEG C, colloidal sol gradually becomes gel, as powder, that is, obtains nanometer
Red schorl phase titanium dioxide.The above method is that colloidal sol (sol) is initially formed after butyl titanate is added, and re-forms gel (gel),
Actually sol-gel process is prepared, and above-mentioned preparation process is relative complex.
The content of the invention
It is an object of the invention to provide a kind of preparation method of rice-shaped red schorl phase titanium dioxide nano particle, the system
Red schorl phase titanium dioxide nano particle purity obtained by Preparation Method preparation is high, and preparation process is relatively easy.
To reach above-mentioned purpose, base case of the invention is as follows：
A kind of preparation method of rice-shaped red schorl phase titanium dioxide nano particle, comprises the following steps：
(1) 14-16g P123 are dissolved in the hydrochloric acid of 460-480ml, the P123- hydrochloric acid solutions that stirring is clarified, institute
The concentration for stating hydrochloric acid is 0.4-0.45mol/L；
(2) in the P123- hydrochloric acid solutions for preparing 51-53g butyl titanates addition step 1, at a temperature of 32-35 DEG C
Stirring hydrolysis 60-75 hours；
(3) the hydrolysis suspension centrifugation obtained after step 2 is hydrolyzed, isolates white solid, and use deionized water rinsing；
(4) white solid that step 3 is obtained is dried at room temperature for, that is, obtains rice-shaped Rutile Type dioxy
Change titanium nano-particle.
The effect of this programme：1st, the use of common butyl titanate is titanium source, in 32-35 DEG C in the hydrochloric acid solution of P123
At a temperature of hydrolyze, hydrolysate is centrifuged, wash after directly obtain single crystalline phase by natural drying at room temperature
Red schorl phase titanium dioxide material, and purity is high, can substantially reach more than 99.9%；2nd, using preparation method of the invention
The red schorl phase titanium dioxide material for obtaining is the nano-particle of highly uniform rice-shaped, size in 80nm × 10nm or so,
Above-mentioned uniform nano-particle need not be classified treatment when in use, compared with the mixed and disorderly nano-particle of size, use valency
Value is higher, such as when the uniform nano-particle of above-mentioned size is as catalyst, can guarantee that the avtive spot of every particle is uniform,
It is very high in research field application value so as to ensure that every catalytic performance of nano-particle is uniform；Size is uniform also as noted above
Nano-particle as catalyst carrier when, can spread the material that is catalyzed uniform, resistance to mass tranfer is uniform, so as to improve catalysis
Effect；3rd, at 30 DEG C or so, preparation process needs not move through the height of any high energy consumption to the hydrolysis temperature in this programme preparation process
The hydrothermal treatment process of warm roasting process or complexity, preparation process is relatively easy, and save energy.
Prioritization scheme 1, the further optimization to base case, the quality of the P123 is 15.5g；Hydrochloric acid volume is
480ml, concentration is 0.43mol/L；The quality of butyl titanate is 52.54g.Inventor is had found by experiment, is matched somebody with somebody using above-mentioned
The purity of the red schorl phase titanium dioxide material that the raw material of ratio is prepared is higher, and nano-particle size uniform.
Prioritization scheme 2, the further optimization to base case, after step 1, the water by P123- hydrochloric acid solutions at 35 DEG C
Stirred 25-35 minutes in bath, stirring frequency is 150-200r/min.P123- hydrochloric acid solutions heat can guarantee that heating in a water bath
Uniformly, and the stirring frequency of above range can make P123- hydrochloric acid solutions more uniform, so that subsequent reactions process is faster,
And after experiment is found through above-mentioned treatment, the purity and uniformity of the nano-particle for preparing increase.
Prioritization scheme 3, to base case, prioritization scheme 1,2 any one further optimization, in step 2, the metatitanic acid four
The addition of butyl ester is added dropwise using glue head dropper 30-40 drops/min, and butyl titanate is being added into P123- hydrochloric acid using aforesaid way
Solution, can make particle evenly.
Prioritization scheme 4, to base case, prioritization scheme 1,2 any one further optimization, stirred in a water bath in step 2
Mix hydrolysis 72 hours.After stirred in water bath hydrolyzes the above-mentioned time, can fully be reacted between raw material, generate more golden red
Stone phase titanium dioxide nano particle.
Brief description of the drawings
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.
Specific embodiment
Below by specific embodiment, the present invention is further detailed explanation：
In following embodiment, mentioned P123 is a kind of triblock copolymer, and full name is:PEO-polycyclic
Ethylene Oxide-PEO triblock copolymer, is a kind of nonionic surfactant.
The method for preparing rice-shaped red schorl phase titanium dioxide nano particle is only illustrated by taking embodiment 1 as an example below,
Other embodiment only lists the difference part with embodiment 1, and all embodiments are represented in table 1.
Embodiment 1
A kind of preparation method of rice-shaped red schorl phase titanium dioxide nano particle, comprises the following steps：
(1) 15.5g P123 are dissolved in the hydrochloric acid of 480ml, the P123- hydrochloric acid solutions that stirring is clarified, the hydrochloric acid
Concentration be 0.43mol/L；
(2) it is 52.54g butyl titanates glue head dropper is molten with the P123- hydrochloric acid that 35 drop/min are added dropwise to step 1 preparation
In liquid, hydrolysis 72 hours is stirred under 35 DEG C of bath temperature；
(3) the hydrolysis suspension obtained after step 2 is hydrolyzed is centrifuged in centrifuge, isolates white solid, and spend
Ionized water is rinsed；
(4) white solid that step 3 is obtained is dried at room temperature for, that is, obtains rice-shaped red schorl phase titanium dioxide nano
Particle.
Embodiment 4
The present embodiment is with the difference part of embodiment 1, after step 1, the water-bath by P123- hydrochloric acid solutions at 35 DEG C
Middle stirring 30 minutes, stirring frequency is 150-200r/min.P123- hydrochloric acid solutions heat can guarantee that homogeneous heating in a water bath,
So that subsequent reactions process is faster, and after experiment is found through above-mentioned treatment, the purity of the nano-particle for preparing and
Even property increases.
Table 1
The rutile-phase nano particle that Example 1-5 is prepared below, detects its purity and particle uniformity respectively,
Wherein uniformity represents that * quantity is more with the quantity of *, represents that nano-particle is more uniform, as a result such as table 2：
Table 2
As can be drawn from Table 2 drawing a conclusion：
1st, embodiment 1 compared with Example 4, difference be embodiment 4 after step 1, by P123- hydrochloric acid solutions 35
DEG C water-bath in moderate-speed mixer 30 minutes.It can thus be seen that by above-mentioned process step, the nanoparticle for preparing can be improved
Sub- purity and particle uniformity；
2nd, the purity of the red schorl phase titanium dioxide nano particle prepared in embodiment 1-5 is pure more than 99%
Degree is very high.
Can by the testing result accompanying drawing 1-5 for observing the red schorl phase titanium dioxide nano particle that embodiment 1 is prepared
Drawn a conclusion with drawing：
1st, 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 this
The transmission electron microscope picture of the titanium dioxide nano-particle material prepared by inventive embodiments 1.This hair is can be seen that with reference to Fig. 1 and Fig. 2
Bright prepared titanium dioxide nano-particle material has the pattern of rice-shaped, and size is in 80nm × 10nm or so.
2nd, the XRD spectra of the titanium dioxide nano-particle material gone out synthesized by Fig. 3 embodiment of the present invention 1.It can be seen that this
The prepared titanium dioxide nano-particle material of invention has the diffraction maximum consistent with red schorl phase titanium dioxide standard items, and this says
Bright its crystalline phase is Rutile Type.Furthermore it is possible to see the XRD spectral peaks of the titanium dioxide nano-particle material prepared by the present invention
Width is substantially bigger than two kinds of width of the XRD spectral peaks of titanium dioxide standard items, and this also illustrates that its particle size is significantly less than two kinds
The particle size of titanium dioxide standard items, and the Electronic Speculum test result of Fig. 1, Fig. 2 matches.
3rd, Fig. 4 be the titanium dioxide nano-particle material prepared by the embodiment of the present invention 1 uv raman spectroscopy figure and can
See Raman spectrogram.The excitation wavelength of visible Raman spectrum test is 532nm, and the excitation wavelength of uv raman spectroscopy test is
325nm, the spectral peak in both Raman spectrograms is all the spectral peak of typical red schorl phase titanium dioxide.Because visible Raman light
Spectrum test is more the information of the inside nanoparticles of reflection, and the test of two uv raman spectroscopies is more the nanoparticle of reflection
The information in sublist face, so with reference to the ultraviolet Raman and visible Raman spectrogram of Fig. 4, it can be appreciated that the embodiment of the present invention 1
Whether inside particles or particle surface are all rutile phases to prepared titanium dioxide nano-particle.
Above-described is only embodiments of the invention, and the general knowledge such as known characteristic does not make excessive description herein in scheme.
It should be pointed out that for a person skilled in the art, without departing from the inventive concept of the premise, some changes can also be made
Shape and improvement, these should also be considered as protection scope of the present invention, these effects and patent for implementing all without the influence present invention
Practicality.This application claims protection domain should be defined by the content of its claim, the specific embodiment party in specification
Formula etc. records the content that can be used for explaining claim.
Claims (5)
1. a kind of preparation method of rice-shaped red schorl phase titanium dioxide nano particle, it is characterised in that comprise the following steps：
（1）14-16g P123 are dissolved in the hydrochloric acid of 460-480mL, the P123- hydrochloric acid solutions that stirring is clarified, the salt
The concentration of acid is 0.4-0.45mol/L；
（2）In the P123- hydrochloric acid solutions for adding step (1) to prepare 51-53g butyl titanates, stirred at a temperature of 32-35 DEG C
Mix hydrolysis 60-75 hours；
（3）The hydrolysis suspension centrifugation obtained after step (2) is hydrolyzed, isolates white solid, and use deionized water rinsing；
（4）The white solid that step (3) is obtained is dried at room temperature for, that is, obtains rice-shaped red schorl phase titanium dioxide nano grain
Son.
2. a kind of preparation method of rice-shaped red schorl phase titanium dioxide nano particle according to claim 1, its feature
It is that the quality of the P123 is 15.5g；Hydrochloric acid volume is 480mL, and concentration is 0.43mol/L；The quality of butyl titanate is
52.54g。
3. a kind of preparation method of rice-shaped red schorl phase titanium dioxide nano particle according to claim 1, its feature
It is that after step (1), by P123- hydrochloric acid solutions stirred in water bath 25-35 minutes of 35 DEG C, stirring frequency is 150-
200r/min。
4. the preparation side of a kind of rice-shaped red schorl phase titanium dioxide nano particle according to claim any one of 1-3
Method, it is characterised in that in step (2), the addition of the butyl titanate is added dropwise using glue head dropper 30-40 drops/min.
5. the preparation side of a kind of rice-shaped red schorl phase titanium dioxide nano particle according to claim any one of 1-3
Method, it is characterised in that stirring is hydrolyzed 72 hours in a water bath in step (2).
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| CN106935843B (en) * | 2017-03-23 | 2020-10-30 | 复旦大学 | Rutile phase nano titanium dioxide and low-temperature preparation method and application thereof |
| 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 |
| 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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| CN100436329C (en) * | 2006-03-03 | 2008-11-26 | 厦门大学 | Process for preparing nano mesoporous titanium dioxide at low tempeature |
| JP6068927B2 (en) * | 2012-10-24 | 2017-01-25 | チタン工業株式会社 | Rutile titanium oxide and cosmetics using the same |
| CN104016405B (en) * | 2014-05-30 | 2016-01-20 | 武汉理工大学 | A kind of flower-shaped mesoporous titanium dioxide material and preparation method thereof and application |
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