CN107226481B - A kind of preparation method of the spherical lanthanium titanate of particle - Google Patents
A kind of preparation method of the spherical lanthanium titanate of particle Download PDFInfo
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- CN107226481B CN107226481B CN201710492809.4A CN201710492809A CN107226481B CN 107226481 B CN107226481 B CN 107226481B CN 201710492809 A CN201710492809 A CN 201710492809A CN 107226481 B CN107226481 B CN 107226481B
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/32—Spheres
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention is a kind of spherical lanthanium titanate preparation method of particle.Steps of the method are: under agitation, 10~20 parts of lanthanum source-water mixed liquids are added in 40~50 portions of titanium source -ol mixed liquors, then sodium hydroxide is added into solution, magnetic agitation 20~30 minutes, then it moves on in reaction kettle, is warming up to 180-220 DEG C, react 3-48 hours；It stands to room temperature, after removing supernatant, sediment fraction is added in the reactor containing 100 parts of hydrochloric acid solutions, stirring is washed after 20~30 minutes, then is centrifuged, and 60-100 DEG C of drying, obtaining white powder is the spherical lanthanium titanate of particle.The method of the present invention simple process and low cost, uniform component, novel in shape.
Description
Technical field
Technical solution of the present invention is related to the titanate of lanthanum, the specifically preparation method of the spherical lanthanium titanate of particle.
Background technique
Lanthanium titanate chemical formula is LaTiO3, belong to ABO3Perovskite structural material cannot be only used for production ferroelectricity grid field effect
Transistor, ferroelectric RAM etc. are answered, is also answered in terms of the sewage containing toxic organic compound matter in photocatalysis and processing
With.
It is more for the research of lanthanium titanate at present, but synthetic method is not easy mostly.(B.Madhavan,A.Ashok,
Dielectric properties of A and B-site doped LaTiO3-δ perovskites synthesised
By sol-gel method, J Sol-Gel Sci Technol, 2015,73,1-8) document reports a kind of sol-gel
Synthetic method, time-consuming for the technology, and process is tedious.(I.A.Mkhalid,Visible light photocatalytic
synthesis of aniline with an Au/LaTiO3nanocomposites,Journal of Alloys and
Compounds 2015,631,298-302) document report it is a kind of using ultrasound prepare lanthanium titanate method, the technique behaviour
Make complexity, needs protective gas.Although lanthanium titanate can be obtained in these existing methods, there is presently no methods to obtain
To the lanthanium titanate of particle spherical morphology.
Summary of the invention
It is an object of the present invention to for complex process, condition existing for current lanthanium titanate synthesis process be harsh and cost compared with
The shortcomings that height or lanthanium titanate synthesis process need high-temperature calcination provides a kind of preparation method of spherical lanthanium titanate of particle.This method
It is spherical that particle is prepared using mixed solvent thermal method in alcohol-water system to change the build environment of product by introducing ethylene glycol
Lanthanium titanate.The method of the present invention simple process and low cost, uniform component, novel in shape.
The technical scheme is that
A kind of spherical lanthanium titanate preparation method of particle, comprising the following steps:
(1) titanium source is dissolved in alcoholic solution, it is 0.04541-0.05677 moles of titanium/liter alcohol titanium source -ol that concentration, which is made,
Mixed liquor, for use；
(2) lanthanum source is dissolved in deionized water, it is 0.1150-0.2309 moles of lanthanum/liter water lanthanum source-water that concentration, which is made,
Mixed liquor, for use；
(3) under agitation, 10~20 parts of lanthanum source-water mixed liquids prepared in step (2) are added to 40~50 parts
In titanium source -ol mixed liquor in step (1), after stirring, then sodium hydroxide is added into solution, magnetic agitation 20~30 minutes,
Obtain third mixed liquor；Wherein, in third mixed liquor, addition amount of sodium hydroxide is 0.8-1 mol/L；
(4) then third mixed liquor obtained in step (3) is moved on in reaction kettle, is warming up to 180-220 DEG C after closed,
Reaction 3-48 hours；
(5) reaction kettle of upper step is stood to room temperature, after removing supernatant, precipitating is added to the salt containing 100 parts of 0.2M
In the reactor of acid solution, stirring is washed after 20~30 minutes, then is centrifuged, and 60-100 DEG C of drying obtains white powder
For the spherical lanthanium titanate of particle；
The number of said components is volume parts, and volume unit used in each step is identical.
Titanium source described in the step (1) is butyl titanate, and alcohol source is ethylene glycol.
Lanthanum source described in the step (2) is lanthanum nitrate hexahydrate.
Substantive distinguishing features of the invention are as follows:
In current techniques, using hydro-thermal method, need to be added the lanthanum source titanium source of isodose under alkaline environment, it is only getable
Product is that chemical formula is La2Ti2O7Lanthanium titanate, and its pattern be sheet；Compared to LaTiO3Lanthanium titanate sees the other of report
Common synthetic method, such as solid state reaction, needing presoma to calcine at high temperature several more than ten hours could form, and time-consuming
And energy consumption is big；To sol-gel method, this method is unable to one-step synthesis product, and process is tedious, formed the process time of gel compared with
It is long, and the step of being also required to calcining gel later；Also just like ultrasonic, it is also desirable to multistep reaction can just obtain sample, and
Reaction process needs carry out under the protective atmospheres such as nitrogen, too strong to reaction environment dependence.And the crucial place of the invention patent
It is the addition of ethylene glycol, changes the build environment of product by introducing ethylene glycol, it is molten using mixing in alcohol-water system
Agent thermal method prepares the spherical lanthanium titanate of particle, to achieve the purpose that control its ingredient and pattern.
The beneficial effects of the present invention are:
1. the spherical lanthanium titanate of the obtained particle of the method for the present invention is the lanthanium titanate for having particle spherical, specific pattern is as schemed
Shown in 2, synthesized lanthanium titanate even particle size is spherical obvious.As shown in Figure 1, product is pure phase lanthanium titanate, and diffraction maximum is non-
It is often clear, sharp, illustrate that lanthanium titanate crystallinity is fine.Relative to the synthetic system of previous pure water, the present invention draws in hydro-thermal method
Ethylene glycol is entered, has changed Crystallization and growing environment, and finally obtained the product of such unique morphology, used in the present invention
The disadvantages of raw material is cheap and easy to get, and overcomes in previous lanthanium titanate synthesis process, complex process, condition harshness and higher cost；With
The shortcomings that overcoming existing lanthanium titanate synthesis process to need high-temperature calcination.
2. in the method for the present invention, using green, alcohol-water preparation system of environmental protection, high-temperature calcination is not necessarily to, without protecting gas
Body reduces production cost, is conducive to nonhazardous scale and is combined to and environmental protection.
3. the method for the present invention is simple, it is conducive to batch production.For this patent using green, it is spherical that easy method obtains particle
Lanthanium titanate.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the spherical lanthanium titanate powder X-ray RD spectrogram of particle in embodiment 1.
Fig. 2 is the spherical lanthanium titanate SEM photograph of particle in embodiment 1.
Specific embodiment
Embodiment 1
(1) 0.8ml butyl titanate (about 0.0023mol) is dissolved in 40ml ethylene glycol solution, is stirred evenly, for use；
(2) 1g (about 0.0023mol) lanthanum nitrate hexahydrate is dissolved in 20ml deionized water, stirring to being completely dissolved,
For use；
(3) under agitation, the reaction liquid prepared in step (2) being added in step (1) with 50~60 seconds
In device, after mixing to solution, 2.4g sodium hydroxide is added, magnetic agitation 30 minutes；
(4) mixture obtained in step (3) is then moved on into reaction kettle, 220 DEG C is warming up to after closed, reaction 24 is small
When；
(5) stoste is stood at room temperature, and after removing supernatant, remaining sediment fraction is added to containing 100ml, 0.2mol/L
Hydrochloric acid solution reactor in, stirring is washed after 30 minutes, then is centrifuged, and 80 DEG C of drying, obtaining white powder is
The spherical lanthanium titanate about 1.1g of grain.
Using the spherical lanthanium titanate of particle prepared by the present invention, X-ray diffraction spectrum analysis is carried out as shown in Figure 1, in figure
Diffraction maximum show that product is pure phase lanthanium titanate, be free of other miscellaneous phases, while these diffraction maximums are clear, sharp, illustrate the metatitanic acid
The crystallinity of lanthanum is fine.By transmission electron microscope observing (as shown in Figure 2), the spherical lanthanium titanate of particle is evenly distributed, and particle size
It is uniform, in dozens to a few hundred nanometers or so.
Embodiment 2
Reaction temperature in embodiment 1 in step (4) is set to 180 DEG C, other steps are the same as embodiment 1.It is same to obtain product
Embodiment 1.
Embodiment 3
Reaction temperature in embodiment 1 in step (4) is set to 200 DEG C, other steps are the same as embodiment 1.It is same to obtain product
Embodiment 1.
Embodiment 4
The reaction time of step (4) in embodiment 1 is adjusted to 3h, other steps are the same as embodiment 1.Product is obtained with implementation
Example 1.
Embodiment 5
The reaction time of step (4) in embodiment 1 is adjusted to 12h, other steps are the same as embodiment 1.Product is obtained with real
Apply example 1.
Embodiment 6
The reaction time of step (4) in embodiment 1 is adjusted to 36h, other steps are the same as embodiment 1.Product is obtained with real
Apply example 1.
Embodiment 7
The reaction time of step (4) in embodiment 1 is adjusted to 48h, other steps are the same as embodiment 1.Product is obtained with real
Apply example 1.
Embodiment 8
The ethylene glycol amount of step (1) in embodiment 1 is set to 45ml, the amount of deionized water of step (2) is set to 15ml, other
Step is the same as embodiment 1.Product is obtained with embodiment 1.
Embodiment 9
The ethylene glycol amount of step (1) in embodiment 1 is set to 50ml, the amount of deionized water of step (2) is set to 10ml, other
Step is the same as embodiment 1.Product is obtained with embodiment 1.
Embodiment 10
Amount of sodium hydroxide in embodiment 1 in step (3) is set to 1.92g, other steps are the same as embodiment 1.Obtain product
With embodiment 1.
Embodiment 11
Amount of sodium hydroxide in embodiment 1 in step (3) is set to 2.88g, other steps are the same as embodiment 1.Obtain product
With embodiment 1.
Embodiment 12
Drying temperature in embodiment 1 in step (5) is set to 60 DEG C, other steps are the same as embodiment 1.Product is obtained with real
Apply example 1.
Embodiment 13
Drying temperature in embodiment 1 in step (2) is set to 100 DEG C, other steps are the same as embodiment 1.It is same to obtain product
Embodiment 1.
Unaccomplished matter of the present invention is well-known technique.
Claims (1)
1. a kind of spherical lanthanium titanate preparation method of particle, it is characterized in that method includes the following steps:
(1) titanium source is dissolved in alcoholic solution, concentration is made as the mixing of 0.04541-0.05677 moles of titanium/liter alcohol titanium source -ol
Liquid, for use；
(2) lanthanum source is dissolved in deionized water, it is 0.1150-0.2309 moles of lanthanum/liter water lanthanum source-water mixing that concentration, which is made,
Liquid, for use；
(3) under agitation, 10~20 parts of lanthanum source-water mixed liquids prepared in step (2) are added to 40~50 parts of steps
(1) in the titanium source -ol mixed liquor in, sodium hydroxide is then added into solution again, magnetic agitation 20~30 minutes, obtains third
Mixed liquor；Wherein, in third mixed liquor, addition amount of sodium hydroxide is 0.8-1 mol/L；
(4) then third mixed liquor obtained in step (3) is moved on in reaction kettle, 180-220 DEG C is warming up to after closed, reaction
3-48 hours；
(5) reaction kettle of upper step is stood to room temperature, after removing supernatant, sediment fraction is added to the salt containing 100 parts of 0.2M
In the reactor of acid solution, stirring is washed after 20~30 minutes, then is centrifuged, and 60-100 DEG C of drying obtains white powder
For the spherical lanthanium titanate of particle；
The number of said components is volume parts, and volume unit used in each step is identical；
Titanium source described in the step (1) is butyl titanate, and alcohol source is ethylene glycol；
Lanthanum source described in the step (2) is lanthanum nitrate hexahydrate.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102062881A (en) * | 2010-11-25 | 2011-05-18 | 福州阿石创光电子材料有限公司 | High refractive index evaporation material lanthanum titanate mixture and preparation method thereof |
| CN106868477A (en) * | 2017-03-12 | 2017-06-20 | 苏州南尔材料科技有限公司 | A kind of method that colloidal sol rubbing method prepares metatitanic acid lanthanum film |
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2017
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102062881A (en) * | 2010-11-25 | 2011-05-18 | 福州阿石创光电子材料有限公司 | High refractive index evaporation material lanthanum titanate mixture and preparation method thereof |
| CN106868477A (en) * | 2017-03-12 | 2017-06-20 | 苏州南尔材料科技有限公司 | A kind of method that colloidal sol rubbing method prepares metatitanic acid lanthanum film |
Non-Patent Citations (2)
| Title |
|---|
| Nanocrystalline titanate powders: Synthesis and mechanisms of perovskite particles formation;V. V. Srdic et al.;《Journal of Optoelectronics and Advanced Materials》;20051231;第7卷(第6期);3005-3013 |
| 钛酸镧钠的溶剂热合成研究;孔新刚 等;《陕西科技大学学报》;20151031;第33卷(第5期);66-69 |
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