CN110272067A - A kind of preparation method being hydrated laminar nano lithium titanate - Google Patents
A kind of preparation method being hydrated laminar nano lithium titanate Download PDFInfo
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Abstract
The invention discloses a kind of preparation method for being hydrated laminar nano lithium titanate, include the following steps: that (1) prepares lithium source aqueous solution;(2) after mixing titanium source presoma with ethyl alcohol, deionized water is added, is precipitated under lasting stirring, obtains solid matter after washed;(3) solid matter prepared by step (2) is mixed with the lithium source aqueous solution that step (1) is prepared, obtains the hydration laminar nano lithium titanate through hydro-thermal reaction and post-processing;The structural formula of the hydration laminar nano lithium titanate is Li1.81H0.19Ti2O5·2H2O.The hydration laminar nano lithium titanate that pattern is uniform, dispersion performance is excellent and object is mutually pure can be prepared in preparation method disclosed by the invention, be conducive to further synthesize the spinel type lithium titanate with good dispersion.
Description
Technical field
The present invention relates to the technical field of inorganic material more particularly to a kind of preparation sides for being hydrated laminar nano lithium titanate
Method.
Background technique
With the increasingly exacerbation of energy and environment problem, Development of Novel green energy resource becomes the work weight of current scientific research personnel
Point.Lithium ion battery is due to long with the service life, the advantages that high temperature resistant, capacity is big, memory-less effect, in electronic equipment, electronic vapour
The fields such as vehicle have a wide range of applications.Spinel type lithium titanate (Li4Ti5O12) have zero during lithium ion intercalation/deintercalation
Strain, electrode potential height (1.55V vs Li+/Li) SEI film not easily generated, safety is good, the advantages such as at low cost, therefore becomes
The research emphasis of current lithium ion battery negative material.
Liquid phase method, if sol-gal process, hydro-thermal method are the common methods of current synthesis lithium titanate.However liquid phase method is difficult to one
Walk the lithium titanate (Li of synthetic spinel type4Ti5O12), but can first obtain a kind of water and layered titanic acid lithium
(Li1.81H0.19Ti2O5·2H2O calcining), then by it is carried out at high temperature completes crystal transfer.Therefore, in order to preferably control point
The pattern of spar type lithium titanate, presoma (Li1.81H0.19Ti2O5·2H2O preparation process) is with regard to particularly important.But current liquid
The synthesis of phase method is generallyd use using ethyl alcohol and water as the solvent-thermal method of solvent, and obtained product dispersibility is poor, and piece and piece usually can
It is layering to form microballoon, and pattern is uneven.
Therefore, it is necessary to propose new solution with regard to the above problem.
Summary of the invention
For above-mentioned technical problem of the existing technology, the invention discloses a kind of systems for being hydrated laminar nano lithium titanate
The hydration laminar nano lithium titanate that pattern is uniform, dispersion performance is excellent and object is mutually pure can be prepared in Preparation Method, be conducive into
One-step synthesis has the spinel type lithium titanate of good dispersion.
Specific technical solution is as follows:
A kind of preparation method being hydrated laminar nano lithium titanate, includes the following steps:
(1) lithium source aqueous solution is prepared;
(2) after mixing titanium source presoma with ethyl alcohol, deionized water is added, is precipitated under lasting stirring, it is washed
After obtain solid matter;
(3) solid matter prepared by step (2) is mixed with the lithium source aqueous solution that step (1) is prepared, through hydro-thermal reaction and
Post-processing obtains the hydration laminar nano lithium titanate;
The structural formula of the hydration laminar nano lithium titanate is Li1.81H0.19Ti2O5·2H2O。
In order to avoid the introducing bring product object of alcohol solvent is mutually impure, the problems such as bad dispersibility, the present invention mentions for the first time
Titanium source presoma is added to out in the mixed system of ethyl alcohol and water and generates precipitating, then by resulting white precipitate is titanium source with solid
The form of state carries out hydro-thermal reaction after mixing with the aqueous solution of lithium source.It is uniform using the obtained product morphology of the method, in water
With in ethyl alcohol all have good dispersibility.
The present invention is by the optimization to preparation process, it is entirely avoided ethyl alcohol is introduced in hydro-thermal reaction.Using to system
Standby technological parameter advanced optimizes, and can be prepared that pattern is uniform, dispersion performance is excellent and object mutually pure (not having miscellaneous phase)
It is hydrated laminar nano lithium titanate.
And pass through comparative test and find, if under identical preparation technology parameter, using preparation process in the prior art, though
So pass through the optimization of technological parameter, the hydration laminar nano lithium titanate of same available no miscellaneous phase, but water in products closes stratiform
The pattern of nano lithium titanate is inhomogenous, and dispersion performance is poor, and being unfavorable for it, further synthesis has the point of good dispersion brilliant
Stone-type lithium titanate.It has also been found that the preparation process is more sensitive to the concentration variation of lithium source, relative to the preparation work in the present invention
Skill, lithium source adjustable range is smaller in the preparation process of the prior art, exceeds the adjustable range, will appear in product apparent miscellaneous
Phase, thus it is more unfavorable for actual production.
In step (1):
Lithium source is selected from lithium hydroxide or a hydronium(ion) lithia;
Preferably, the concentration of the lithium source aqueous solution is 0.175~0.225mol/L, it is found through experiment that, the concentration of lithium source
Selection it is most important to the hydration laminar nano lithium titanate that can obtain pure phase.When the concentration of lithium source aqueous solution is too low, can lead
Cause anatase titania miscellaneous phase occur in product;When the excessive concentration of lithium source aqueous solution, product is no longer just that hydration stratiform is received
Rice lithium titanate.
In step (2):
The titanium source presoma is selected from titanate ester, preferably butyl titanate.
Preferably, the volume ratio of the ethyl alcohol and water is 1~5:1;Further preferably 2:1.
Preferably, the amount Yu volume ratio of the substance of the titanium source presoma and ethyl alcohol are 0.1~1mol/L;Further preferably
For 0.5mol/L.
In step (3):
Preferably, the mass volume ratio of the solid matter and the lithium source aqueous solution is 42.5~47.5g/L;Further
Preferably 45~47.5g/L.
Preferably, the solid matter and the lithium source aqueous solution are vigorously stirred 10 to 20min on magnetic agitation platform
Carry out hydro-thermal reaction again afterwards.
Preferably, the temperature of the hydro-thermal reaction is 180~200 DEG C.It is found through experiment that in addition to lithium source concentration, it is also necessary to
The temperature for controlling the hydro-thermal reaction simultaneously can be prepared that pattern is uniform, dispersion performance is excellent in the range of above-mentioned optimization
Different and mutually pure object hydration laminar nano lithium titanate.It is found through experiment that hydrothermal temperature is too low, in the product being prepared
With the presence of more little particle;Hydrothermal temperature is excessively high, and the generation of other miscellaneous phases is had in product.
Preferably, the post-processing includes washing, drying.The drying temperature be 60~80 DEG C, drying time be 8~
12h。
Further preferably:
The concentration of the lithium source aqueous solution is 0.175~0.225mol/L;
The amount of the substance of the titanium source presoma and ethyl alcohol and volume ratio are 0.5mol/L, and the volume ratio of ethyl alcohol and water is 2:
1;
The mass volume ratio of the solid matter and the lithium source aqueous solution is 45~47.5g/L;
The temperature of the hydro-thermal reaction is 180~200 DEG C.
It is found through experiment that it is uniform using the product morphology of the above-mentioned technological parameter preparation advanced optimized, and dispersion performance
Most preferably, be conducive to further synthesize the spinel type lithium titanate with good dispersion.
Compared with prior art, the beneficial effects of the present invention are:
The present invention takes water as a solvent, and using the hydrolytic precipitation of butyl titanate as titanium source, carries out in aqueous solution with lithium source
Hydro-thermal reaction is successfully prepared hydration layered titanic acid lithium.Compared with traditional solvent thermal process, technical solution of the present invention preparation
Product miscellaneous phase it is few, pattern is uniform, while possessing better dispersibility.Better dispersibility means more in electrochemical system
Big specific surface area, shorter ion spread free path, also bring along better chemical property.Therefore the tool that the present invention synthesizes
There is the presoma of good dispersion to there is the metatitanic acid lithium electrode of excellent chemical property to be of great significance synthesis.
Detailed description of the invention
Fig. 1 is the XRD diagram that embodiment 1 prepares product;
Fig. 2 is the SEM photograph that embodiment 1 prepares product;
Fig. 3 is the XRD diagram that comparative example 1 prepares product;
Fig. 4 is the SEM photograph that comparative example 1 prepares product;
Fig. 5 is the XRD diagram that comparative example 2 prepares product;
Fig. 6 is the XRD diagram that comparative example 3 prepares product;
Fig. 7 is the XRD diagram that embodiment 2 prepares product;
Fig. 8 is that embodiment 2 prepares SEM photograph of the product under different amplification;
Fig. 9 is the XRD diagram that comparative example 4 prepares product;
Figure 10 is the SEM photograph that comparative example 4 prepares product;
Figure 11 is the XRD diagram that comparative example 5 prepares product;
Figure 12 is the SEM photograph that comparative example 5 prepares product;
Figure 13 is the XRD diagram that comparative example 6 prepares product.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
(1) mono- hydronium(ion) lithia of 7mmol is added under stiring in 40mL deionized water and forms solution.
(2) 1.7mL (5mmol) butyl titanate is added drop-wise in 10mL ethyl alcohol with liquid-transfering gun, it is immediately molten to ethyl alcohol
5mL deionized water is added dropwise in liquid to form white precipitate and continue to stir;By precipitating, with deionized water centrifuge washing, (revolving speed is
8000rpm) twice.
(3) 1.8g precipitating is added in the aqueous solution of a hydronium(ion) lithia, it will be after stirring after strong stirring 10min
Mixture is poured into the ptfe autoclave of 50mL, reacts 36h at 180 DEG C;After reaction by product spend from
Sub- water with each centrifuge washing of ethyl alcohol three times, dry 12 hours obtain final product at 80 DEG C.
Fig. 1 is the XRD diagram of product manufactured in the present embodiment, can confirm that product is Li from Fig. 11.81H0.19Ti2O5·2H2O,
The object of product is mutually pure not to have miscellaneous phase.
Fig. 2 is the SEM photograph of product manufactured in the present embodiment, and as can be seen from Figure 2, product is in nano-sheet, pattern rule
Then, uniform, good dispersion.
Comparative example 1
It is specific as follows using preparation process in the prior art:
(1) solution is formed into 20mL deionized water by mono- hydronium(ion) lithia of 7mmol is molten under stiring.
(2) 1.7mL butyl titanate is added in 20mL ethyl alcohol, by the ethyl alcohol of butyl titanate under strong stirring
Solution is added in the aqueous solution of a hydronium(ion) lithia and continues to stir 2h, obtains mixed solution.
(3) mixed solution is added in the reaction kettle of 50mL, isothermal reaction 36h at 180 DEG C.After reaction by product
With deionized water and each centrifuge washing of ethyl alcohol three times, dry 12h obtains product at 80 DEG C.
Fig. 3 is the XRD diagram that this comparative example prepares product, and product is the Li of pure phase as can be seen from FIG.1.81H0.19Ti2O5·
2H2O。
Fig. 4 is the SEM photograph that this comparative example prepares product, it has been observed that product morphology is not uniform enough with size, dispersion
Property is poor.
Comparative example 2
Preparation process is identical with embodiment 1, and difference is only that the addition of a hydronium(ion) lithia in step (1)
Amount is adjusted to 4mmol, and the technological parameter of other steps is identical.
Fig. 5 is that this comparative example prepares the XRD diagram of product, it has been observed that occurring Detitanium-ore-type TiO in product2Miscellaneous phase.
Comparative example 3
Preparation process is identical with embodiment 1, and difference is only that the addition of a hydronium(ion) lithia in step (1)
Amount is adjusted to 12mmol, and the technological parameter of other steps is identical.
Fig. 6 is the XRD diagram that this comparative example prepares product, it has been observed that product is LiTiO2, do not observe
Li1.81H0.19Ti2O5·2H2The characteristic peak of O.
Embodiment 2
(1) mono- hydronium(ion) lithia of 9mmol is added under stiring in 40mL deionized water and forms solution.
(2) 1.7mL butyl titanate is added drop-wise in 10mL ethyl alcohol with liquid-transfering gun, is immediately added dropwise into ethanol solution
5mL deionized water forms white precipitate and continues to stir;By precipitating deionized water centrifuge washing (revolving speed 8000rpm) two
Time.
(3) 1.9g precipitating is added in the aqueous solution of a hydronium(ion) lithia, it will be after stirring after strong stirring 10min
Mixture is poured into the ptfe autoclave of 50mL, reacts 36h at 200 DEG C;After reaction by product spend from
Sub- water is with each centrifuge washing of ethyl alcohol three times, the obtained final product after dry 12 hours at 80 DEG C.
Fig. 7 is the XRD diagram that the present embodiment prepares product, it has been observed that product manufactured in the present embodiment is
Li1.81H0.19Ti2O5·2H2O, product object is mutually pure not to have miscellaneous phase.
Fig. 8 is that the present embodiment prepares SEM photograph of the product under different amplification, it has been observed that product is in nanometer sheet
Shape, dispersibility is preferably;It can be seen that surface is smooth from SEM photograph (b) figure of amplification, lamella is completely remained
Shape structure.
Comparative example 4
It is specific as follows using preparation process in the prior art:
(1) solution is formed into 20mL deionized water by mono- hydronium(ion) lithia of 9mmol is molten under stiring.
(2) 1.7mL butyl titanate is added in 20mL ethyl alcohol, by the ethyl alcohol of butyl titanate under strong stirring
Solution is added in the aqueous solution of a hydronium(ion) lithia and continues to stir 2h, obtains mixed solution.
(3) mixed solution is added in the reaction kettle of 50mL, isothermal reaction 36h at 200 DEG C.After reaction by product
With deionized water and each centrifuge washing of ethyl alcohol three times, dry 12h obtains product at 80 DEG C.
Fig. 9 is the XRD diagram that this comparative example prepares product, it has been observed that product is LiTiO2。
Figure 10 is the SEM photograph that this comparative example prepares product, it has been observed that product is short grained accumulation.
Comparative example 5
Preparation process is identical with embodiment 2, and difference, which is only that, is adjusted to hydrothermal temperature in step (3)
160 DEG C, the technological parameter of other steps is identical.
Figure 11 is the XRD diagram that this comparative example prepares product, it has been observed that product is Li1.81H0.19Ti2O5·2H2O。
Figure 12 is the SEM photograph that this comparative example prepares product, it has been observed that the surface of nanometer sheet is more coarse in product,
With the presence of more little particle, it may be possible to since lower reaction temperature slows down the speed of growth of nanometer sheet, cause to have small
Particle is not grown up also in flakes.
Comparative example 6
Preparation process is identical with embodiment 2, and difference, which is only that, is adjusted to hydrothermal temperature in step (3)
220 DEG C, the technological parameter of other steps is identical.
Figure 13 is the XRD diagram that this comparative example prepares product, it has been observed that main phase is Li in product1.81H0.19Ti2O5·
2H2O, but have a small amount of LiTiO2The presence of miscellaneous phase.
Claims (8)
1. a kind of preparation method for being hydrated laminar nano lithium titanate, which comprises the steps of:
(1) lithium source aqueous solution is prepared;
(2) after mixing titanium source presoma with ethyl alcohol, deionized water is added, is precipitated under lasting stirring, is obtained after washed
To solid matter;
(3) by step (2) prepare solid matter mixed with the lithium source aqueous solution that step (1) is prepared, through hydro-thermal reaction and after
Reason obtains the hydration laminar nano lithium titanate;
The structural formula of the hydration laminar nano lithium titanate is Li1.81H0.19Ti2O5·2H2O。
2. the preparation method of hydration laminar nano lithium titanate according to claim 1, which is characterized in that in step (1):
Lithium source is selected from lithium hydroxide or a hydronium(ion) lithia;
The concentration of the lithium source aqueous solution is 0.175~0.225mol/L.
3. the preparation method of hydration laminar nano lithium titanate according to claim 1, which is characterized in that in step (2):
The titanium source presoma is selected from titanate ester;
The volume ratio of the ethyl alcohol and deionized water is 1~5:1;
The amount and volume ratio of the substance of the titanium source presoma and ethyl alcohol are 0.1~1mol/L.
4. the preparation method of hydration laminar nano lithium titanate according to claim 3, which is characterized in that the titanate ester
Selected from butyl titanate.
5. the preparation method of hydration laminar nano lithium titanate according to claim 1, which is characterized in that in step (3):
The mass volume ratio of the solid matter and the lithium source aqueous solution is 42.5~47.5g/L.
6. the preparation method of hydration laminar nano lithium titanate according to claim 1, which is characterized in that in step (3), institute
The temperature for stating hydro-thermal reaction is 180~200 DEG C.
7. the preparation method of hydration laminar nano lithium titanate according to claim 1, which is characterized in that in step (3), institute
Stating post-processing includes washing, drying.
8. the preparation method of hydration laminar nano lithium titanate according to claim 1, it is characterised in that:
The concentration of the lithium source aqueous solution is 0.175~0.225mol/L;
The amount of the substance of the titanium source presoma and ethyl alcohol and volume ratio are 0.5mol/L, and the volume ratio of ethyl alcohol and water is 2:1;
The mass volume ratio of the solid matter and the lithium source aqueous solution is 45~47.5g/L;
The temperature of the hydro-thermal reaction is 180~200 DEG C.
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