CN110040770A - A kind of method that microchannel continuity method prepares nano-level sphere barium titanate - Google Patents
A kind of method that microchannel continuity method prepares nano-level sphere barium titanate Download PDFInfo
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- CN110040770A CN110040770A CN201910495454.3A CN201910495454A CN110040770A CN 110040770 A CN110040770 A CN 110040770A CN 201910495454 A CN201910495454 A CN 201910495454A CN 110040770 A CN110040770 A CN 110040770A
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
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- C01G23/006—Alkaline earth titanates
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention relates to a kind of methods that microchannel continuity method prepares nano-level sphere barium titanate, comprising: following steps: (1) preparing Ba solution, Ti solution and lye；(2) mixed liquor of Ba liquid and Ti liquid, lye are squeezed into T-type or Y type mixer, are reacted at a given temperature, and mixer has the microchannel of internal diameter 0.5-1mm.This method improves spherical shape BaTiO3The pattern and particle size of powder, to perform place mat for industrial continuous production.
Description
Technical field
The invention belongs to spherical barium titanate preparation fields more particularly to a kind of microchannel continuity method to prepare nano-level sphere titanium
The method of sour barium.
Background technique
Barium titanate (BaTiO with perovskite structure3) other than with electrology characteristics such as dielectric, piezoelectricity, also have good
The features such as good biocompatibility, high reflectance, Gao Baidu, microcosmic uniform particle diameter can be used as quickly detecting human health
The raw material of the medicine dry plate diffusion layer of index.Therefore, preparing spherical barium carbonate powder is the key that medical science application skill
One of art.
Currently, solid phase method and liquid phase method are to prepare BaTiO3The main method of powder.Solid phase method prepares BaTiO3It is to pass through original
Expect BaCO3And TiO2It synthesizes at high temperature, which has been used for industrialized production, but the difficult uniform regular spherical BaTiO of formation3, produce
Object is mostly irregular pattern rambunctious.Liquid phase method mainly has hydro-thermal method, sol-gel method, the precipitation method, microemulsion method etc..Water
Thermal method prepares BaTiO3Required equipment requirement is higher, and technical difficulty is larger.The easy moisture absorption water of the alkoxide that sol-gel method uses
Solution, and cost of material is higher, reaction time is long, is unfavorable for industrialized production；The cost of material relative moderate that the precipitation method use, system
Standby technique is simple with respect to hydro-thermal method, sol-gel method, but the preparation of its precipitation method mostly uses batch process to operate greatly, the behaviour such as loading and unloading
Make complex, procedure parameter is not easy to control.In view of these factors, the present invention is prepared using a kind of microchannel continuous precipitation
Nano-level sphere BaTiO3, improve the problems such as periodic precipitation method is cumbersome.
The basic principle of the precipitation method is to mix different material under solution state, and corresponding precipitating reagent system is added thereto
It is standby to obtain the precursor precipitate of particle, then be dried or calcine to obtain corresponding powder.Ding Shiwen etc. is with Ba (OH)2With
TiCl4For raw material, the BaTiO for using a step precipitation method to be prepared into partial size as 50-80nm3Powder.Hu etc. is on the basis of co-precipitation
On, with Ba (OH)2、BaCl2And TiCl4It is sky with hydroxypropyl cellulose (HPC) using isopropanol and water mixed solvent for raw material
Between dispersing agent be prepared into monodisperse BaTiO3Particle.But the periodic precipitation method has some limitations in operation, such as
Process conditions are not easy to control etc..
Microchannel method unique advantage possessed by it is reacted, quickly, efficiently such as mass-and heat-transfer, process equipment is simple,
Easily-controlled reaction conditions etc., it is easy to industrialized production convenient for directly amplifying operation.Combine liquid phase method using micro- logical both at home and abroad at present
The research of road technology synthesis different materials has very much, there is inorganic particulate material, semiconductor and polymer material etc..But it is right both at home and abroad
Nanometer BaTiO is prepared in microchannel3Research it is less, therefore develop the technology that a kind of microchannel continuity method prepares barium titanate
Have great importance.
Continuity method produces BaTiO3Technique only has a small amount of scholar at present and is studied.It is " a kind of continuously to prepare barium titanate powder
It is disclosed in the technique of body " (CN 101434407) a kind of using continuous synthesis reactor preparation BaTiO3Technology of preparing, by
Relatively complicated in its material feeding operation, the 20-30mm of the minimum heating part of the reactor inside diameter of use, is inner port
Temperature is higher than the double pipe heat exchanger of 180 DEG C of conduction oils, and material need to stop 150-300min in insulating sections reaction tube, instead
Answer the period longer.Bowen etc. is in " Synthesis of barium titanate powders by low-temperature
aqueous synthesis using a new segmented flow tubular reactor”(Key Engineering
Materials, vol 206 (2002)) report is using low temperature Aqueous phase, respectively in batch reactor and segmented flow pipe reaction
BaTiO is synthesized in device (SFTR)3Powder, discovery use Y type mixer, N at 95 DEG C2For disjunction stream, pass through internal diameter 4mm, long 12m
Tubular reactor (residence time 10min) after obtained product BaTiO3There is 80% grain diameter to be less than 100nm in powder, and
Only 57% grain diameter is in 100nm or less in batch reactor.
The above continuity method prepares BaTiO3Research usually choose the reactor of internal diameter 4mm or more, obtained product is also simultaneously
It is not limited to spherical morphology, and reaction time is longer, therefore, is improved on the basis of continuity method, to improve product
BaTiO3Pattern and partial size, shorten the reaction time, this for industrialization continuous production application play a crucial role.
Summary of the invention
Technical problems to be solved by the inivention
The application uses the spherical BaTiO of microchannel continuity method new technology synthesis nano size tunable3, shorten reaction week
Phase accelerates its reaction efficiency, is conducive to industrialize continuous production.
Method for solving technical problem
An embodiment according to the present invention provides a kind of microchannel continuity method and prepares ball shaped nano grade barium carbonate powder
Method, comprising the following steps: (1) prepare Ba liquid, Ti liquid and lye；(2) mixed liquor of Ba liquid and Ti liquid is squeezed into lye
It in mixer, is reacted at a given temperature, mixer has the microchannel of internal diameter 0.5-1mm, and mixer is T-type mixer
Or Y type mixer, giving reaction temperature is 85~95 DEG C.
A kind of embodiment be further include separation, drying steps after reaction.
A kind of embodiment is that the Ba liquid is BaCl2、Ba(OH)2Aqueous solution；The Ti liquid is TiCl4、TiOCl2
Aqueous solution.
A kind of embodiment is that the concentration of Ba ion is 0.10~0.50mol/L in the Ba liquid, in the Ti liquid Ti from
The concentration of son is 0.10~0.50mol/L, and the molar ratio of Ba ion and Ti ion is 1.0~1.2 in mixed liquor.
A kind of embodiment is that the lye is the aqueous solution of NaOH, KOH, and the concentration of lye is 2~5mol/L.
A kind of embodiment is that the preparation temperature of Ti liquid is the ice-water bath lower than 4 DEG C in step (1).
A kind of embodiment is that the material of mixer microchannel is stainless steel.
A kind of embodiment is that the mixed liquor of Ba liquid and Ti liquid and the feed rate of lye are identical, and is 1~5mL/min.
Invention effect
The advantage of the invention is that innovated on the continuity method design scheme of microchannel, using T-type or Y type mixer,
Two kinds of materials are squeezed into microchannel plate simultaneously by constant-flux pump to answer in pipeline, reaction solution is gradually heated to 90 DEG C instead in pipeline
It answers, by controlling differential responses condition, the spherical BaTiO of size tunable is obtained from tube outlet3。
From the description of following exemplary embodiment, further characteristic of the invention will become obvious.
Detailed description of the invention
Fig. 1 is product BaTiO3The XRD spectra of powder；
Wherein (a) is the barium titanate XRD spectra of standard card PDF#31-0174；It (b) is obtained under the conditions of embodiment 2
Barium titanate XRD spectra.
Fig. 2 is to be prepared into BaTiO3SEM figure；
Wherein Fig. 2 (a) is the resulting BaTiO of embodiment 13SEM figure, Fig. 2 (b) be the resulting BaTiO of embodiment 23's
SEM figure, Fig. 2 (c) are the resulting BaTiO of embodiment 33SEM figure, Fig. 2 (d) be the resulting BaTiO of embodiment 43SEM figure, figure
2 (e) be the resulting BaTiO of embodiment 53SEM figure.
Specific embodiment
An embodiment of the disclosure is specifically described below, but the disclosure is not limited to this.
In above-mentioned preparation BaTiO3Method in, spherical BaTiO is controlled by regulation reaction condition3Partial size.Micro- logical
Road continuous precipitation prepares BaTiO3Reaction in, alkaline environment be generate stablize BaTiO3Essential condition, certain
BaTiO under the conditions of alkali concentration3It can be stabilized, and due to BaTiO when alkali concentration is lower3Formation lack enough motive forces, make
The conversion of other forms can be carried out by obtaining product, lead to BaTiO3Purity reduces.In addition, the feed flow of material and the alkali dense of system
Degree can all generate certain influence to the partial size of spherical BaTiO3.When flow is larger also not due to the mixed liquor in microchannel tubing
It is uniformly mixed and is flowed out from tube outlet, the product grain resulted in is imperfect；As flow reduces, micro passage reaction
Middle reaction solution is mixed during tube runs, and microcosmic mixability is reinforced, and mass-transfer efficiency is improved, is formed more
Barium titanate nucleus, partial size reduce.And the alkali concentration of system increases, so that the OH- in solution increases, in reaction solution in the short period
A large amount of BaTiO3 nucleus can be formed, the rate that solute is spread from bulk solution to BaTiO3 plane of crystal at this time reduces, particle
Growth is restricted, and the barium titanate particles resulted in reduce.Therefore the present invention is connected by T-type or Y type mixer and microchannel
The design scheme of continuous method controls the alkali concentration of flow and system, to improve spherical BaTiO3The pattern and partial size of powder
Size, to perform place mat for industrial continuous production.
Preparation for Ti liquid: it is optional, by TiCl under ice-water bath stirring condition4It is added dropwise in deionized water, mixes
It closes uniform；
Ba liquid is prepared: it is optional, weigh a certain amount of BaCl2·2H2O solid powder is added and Ti liquid in beaker
The deionized water dissolving of equivalent, stirs and evenly mixs；
For the mixed liquor of Ba liquid and Ti liquid: the former two kinds of solution are stirred and evenly mixed, it is spare；
For Alkali liquid compounding: taking appropriate sodium hydrate solid particle in beaker, under agitation addition and mixed liquor
The deionized water dissolving of equivalent controls aqueous slkali initial concentration 2-5mol/L, is cooled to room temperature, spare；
Mixed liquor and lye are passed through into constant-flux pump respectively, control different flow 1-5mL/min squeezes into T-type or Y type mixer
In, the stainless steel micro pipe road of internal diameter 0.5-1mm is flowed through, is reacted.
Centrifuge washing is carried out for several times after collecting via the white solid precipitating of microchannel reaction tube outflow, is placed in 80 DEG C of baking ovens
Middle drying.
Using the above operating method step, the spherical BaTiO that average grain diameter is 40nm-200nm can be obtained3Particle, with reality
The controllable preparation of existing partial size and continuous production.
Embodiment
Experiment uses cheap soluble barium salt for BaCl2·2H2O is analyzed pure；Soluble titanium salt is TiCl4, point
It analyses pure；Precipitating reagent used is NaOH, is analyzed pure；90 DEG C are set by water bath with thermostatic control before experiment.
Example 1
3mol/L NaOH solution is stirred evenly and is cooled to room temperature, as A liquid.Meanwhile preparing 0.15mol/L BaCl2
Solution；According to Ba/Ti molar ratio 1.10, by TiCl under ice-water bath stirring condition4It is added dropwise in deionized water, obtains equivalent
Ti liquid, then the two is uniformly mixed, obtains B liquid.A, B liquid are squeezed into T-type by constant-flux pump with the flow of 1mL/min respectively to mix
In clutch, the microchannel tubing of long 5m internal diameter 1mm is flowed through, the white precipitate obtained at tube outlet is centrifuged, is washed for several times
12h is dried after washing in 80 DEG C of baking ovens, obtains the spherical BaTiO of average grain diameter 40nm3Powder.
Example 2
3mol/L NaOH solution is stirred evenly and is cooled to room temperature, as A liquid.Meanwhile preparing 0.15mol/L BaCl2
Solution；According to Ba/Ti molar ratio 1.0, by TiCl under ice-water bath stirring condition4It is added dropwise in deionized water, obtains equivalent
Ti liquid, then the two is uniformly mixed, obtains B liquid.A, B liquid are squeezed into T-type by constant-flux pump with the flow of 2mL/min respectively to mix
In clutch, the microchannel tubing of long 5m internal diameter 0.5mm is flowed through, the white precipitate obtained at tube outlet is centrifuged, for several times
12h is dried after washing in 80 DEG C of baking ovens, obtains the spherical BaTiO of average grain diameter 100nm3Powder.
Example 3
3mol/L NaOH solution is stirred evenly and is cooled to room temperature, as A liquid.Meanwhile preparing 0.15mol/L BaCl2
Solution；According to Ba/Ti molar ratio 1.2, by TiCl under ice-water bath stirring condition4It is added dropwise in deionized water, obtains equivalent
Ti liquid, then the two is uniformly mixed, obtains B liquid.A, B liquid are squeezed into T-type by constant-flux pump with the flow of 3mL/min respectively to mix
In clutch, the microchannel tubing of long 5m internal diameter 1mm is flowed through, the white precipitate obtained at tube outlet is centrifuged, is washed for several times
12h is dried after washing in 80 DEG C of baking ovens, obtains the spherical BaTiO of average grain diameter 180nm3Powder.
Example 4
2mol/L NaOH solution is stirred evenly and is cooled to room temperature, as A liquid.Meanwhile preparing 0.15mol/L BaCl2
Solution；According to Ba/Ti molar ratio 1.11, by TiCl under ice-water bath stirring condition4It is added dropwise in deionized water, obtains equivalent
Ti liquid, then the two is uniformly mixed, obtains B liquid.A, B liquid are squeezed into T-type by constant-flux pump with the flow of 2mL/min respectively to mix
In clutch, the microchannel tubing of long 5m internal diameter 0.5mm is flowed through, the white precipitate obtained at tube outlet is centrifuged, for several times
12h is dried after washing in 80 DEG C of baking ovens, obtains the spherical BaTiO of average grain diameter 180nm3Powder.
Example 5
5mol/L NaOH solution is stirred evenly and is cooled to room temperature, as A liquid.Meanwhile preparing 0.15mol/L BaCl2
Solution；According to Ba/Ti molar ratio 1.150, by TiCl under ice-water bath stirring condition4It is added dropwise in deionized water, obtains
The two, is then uniformly mixed by the Ti liquid of amount, obtains B liquid.A, B liquid are squeezed into T-type by constant-flux pump with the flow of 2mL/min respectively
In mixer, the microchannel tubing of long 5m internal diameter 1mm is flowed through, the white precipitate obtained at tube outlet is centrifuged, for several times
12h is dried after washing in 80 DEG C of baking ovens, obtains the spherical BaTiO of average grain diameter 90nm3Powder.
Using XRD-7000 type Rigaku Co., Ltd. X-ray diffractometer (X-ray diffractometer, XRD) point
The object phase composition for analysing barium titanate sample radiates, 40kV and 30mA in CuK α,With 4 ° of min-1Scanning speed
Rate obtains XRD spectrum；Using ZEISS-SUPRA55 type field emission scanning electron microscope (Scanning electron
Microcopy, SEM) observe Product samples surface topography and partial size.Using TENSOR-27 type infrared spectrometer (FT-IR)
Sample is tested and analyzed, in 400~4000cm-1It is scanned in wave-length coverage, resolution ratio 8cm-1.By BaTiO3/KBr
Mass ratio 1/100 carries out tabletting.
Fig. 1 show the BaTiO that embodiment 2 obtains3The XRD diagram of sample, (a) is standard card PDF#31-0174 in figure
Cubic phase barium titanate XRD spectra, be (b) XRD spectra for the barium titanate sample being prepared under the conditions of embodiment 2.Occur in figure
BaTiO3Characteristic diffraction peak, each main diffraction peak position is consistent with standard spectrogram PDF#31-0174, illustrates that the sample is
Resulting BaTiO3Crystal.
As shown in Fig. 2, for the SEM figure of embodiment 1, embodiment 2, embodiment 3, embodiment 4 and embodiment 5.This experiment institute
The product obtained is the BaTiO of the spherical morphology of uniform particle diameter3。
This experiment combines T-type or Y type mixer, develops a kind of microchannel continuity method and prepares nano-level sphere BaTiO3Powder
New technology.Reaction solution is gradually heated to given 85~95 DEG C of reaction temperature in pipeline in flow process (molten when temperature is too low
The Ti-O polymerization jelly and Ba formed in liquid2+Between do not obtain can react to each other collision be nucleated required for energy, cause
Product lattice is imperfect, haves the defects that certain), it is resulting product in the sample that exit is collected, substantially reduces anti-
It answers the period, and is prepared into the nano-level sphere pattern BaTiO of size tunable3Particle, more conducively industrialization continuous production, and be electricity
The application in the fields such as, optics, medicine provides more choices space.
This embodiment is merely preferred embodiments of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with scope of protection of the claims
Subject to.
Claims (8)
1. a kind of method that microchannel continuity method prepares nano-level sphere barium titanate characterized by comprising following steps:
(1) Ba solution, Ti solution and lye are prepared；
(2) mixed liquor of Ba liquid and Ti liquid and lye are squeezed into mixer, are reacted at a given temperature, and mixer has interior
The microchannel of diameter 0.5-1mm, mixer are T-type mixer or Y type mixer, and giving reaction temperature is 85~95 DEG C.
2. method according to claim 1, wherein further include separation, drying steps after reaction.
3. any one of -2 the method according to claim 1, wherein the Ba liquid is BaCl2、Ba(OH)2Aqueous solution；It is described
Ti liquid is TiCl4、TiOCl2Aqueous solution.
4. any one of -3 the methods according to claim 1, wherein in the Ba liquid concentration of Ba ion be 0.10~
0.50mol/L, the concentration of Ti ion is 0.10~0.50mol/L in the Ti liquid, and Ba ion and Ti ion rubs in mixed liquor
You are than being 1.0~1.2.
5. any one of -4 the methods according to claim 1, wherein the lye is the aqueous solution of NaOH, KOH, lye it is dense
Degree is 2~5mol/L.
6. any one of -5 the method according to claim 1, wherein the preparation temperature of Ti liquid is the ice lower than 4 DEG C in step (1)
Water-bath.
7. any one of -6 the method according to claim 1, wherein the material of mixer microchannel is stainless steel.
8. any one of -7 the method according to claim 1, wherein the feed rate phase of the mixed liquor of Ba liquid and Ti liquid and lye
It together, and is 1~5mL/min.
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| CN110776913A (en) * | 2019-11-21 | 2020-02-11 | 上海大学(浙江·嘉兴)新兴产业研究院 | BaTiO 3Preparation method of quantum dots |
| WO2022107695A1 (en) * | 2020-11-19 | 2022-05-27 | 日本化学工業株式会社 | Method for producing barium titanyl oxalate and method for producing barium titanate |
| JP2022081058A (en) * | 2020-11-19 | 2022-05-31 | 日本化学工業株式会社 | Method for producing barium titanyl oxalate and method for producing barium titanate |
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| JP2022081058A (en) * | 2020-11-19 | 2022-05-31 | 日本化学工業株式会社 | Method for producing barium titanyl oxalate and method for producing barium titanate |
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Application publication date: 20190723 |