CN111573717B - Method for preparing high-purity nano lithium titanate from industrial metatitanic acid - Google Patents

Method for preparing high-purity nano lithium titanate from industrial metatitanic acid Download PDF

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CN111573717B
CN111573717B CN202010467709.8A CN202010467709A CN111573717B CN 111573717 B CN111573717 B CN 111573717B CN 202010467709 A CN202010467709 A CN 202010467709A CN 111573717 B CN111573717 B CN 111573717B
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lithium titanate
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马光强
程敏
刘蓉
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Panzhihua University
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    • H01—ELECTRIC ELEMENTS
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Abstract

The invention belongs to the field of lithium battery materials, and particularly relates to a method for preparing high-purity nano lithium titanate from industrial metatitanic acid. The invention aims to solve the technical problem of providing a method for preparing high-purity nano lithium titanate from industrial metatitanic acid, which comprises the following steps: A. mixing industrial metatitanic acid, hydrogen peroxide and ammonia water, and reacting at 0-5 ℃ to obtain a mixed solution; B. heating the mixed solution, dropwise adding a lithium source and a dispersing agent into the mixed solution, heating to 60-80 ℃, and keeping the temperature; C. and after the heat preservation is finished, separating, washing, drying and calcining the solid to obtain the high-purity nano lithium titanate. The method can prepare the high-purity nano lithium titanate by taking the industrial metatitanic acid as a raw material.

Description

Method for preparing high-purity nano lithium titanate from industrial metatitanic acid
Technical Field
The invention belongs to the field of lithium battery materials, and particularly relates to a method for preparing high-purity nano lithium titanate by taking industrial metatitanic acid as a raw material.
Background
Spinel type Li 4 Ti 5 O 12 The lithium ion battery cathode material is a novel lithium ion battery cathode material, has no volume change in the lithium ion de-intercalation process, has the advantages of super-long cycle life, excellent safety performance, low-temperature workability and the like, and has generally good market application potential in the field of lithium ion batteries. But is limited by factors such as high purity requirement on raw materials, high synthesis cost, low product capacity and the like, and is not applied to the field of lithium ion batteries on a large scale at present.
CN 105280908B discloses a method for preparing lithium titanate by using sulfuric acid process titanium dioxide intermediate product industrial metatitanic acid, which comprises the steps of pretreating the intermediate product industrial metatitanic acid in the production process of sulfuric acid process titanium dioxide, removing impurities mixed with the intermediate product industrial metatitanic acid, dehydrating and drying, adding lithium salt for soaking and curing, and finally heating and calcining to synthesize lithium titanate. The method has two defects, namely, the industrial metatitanic acid needs to be pretreated to remove impurities such as sulfate radicals and metal ions, but the industrial metatitanic acid has strong adsorbability due to large specific surface area, and the final product performance is influenced due to limited impurity removal effect only by simple washing; secondly, the hydrolyzed industrial metatitanic acid has larger particle size, the solid phase method is directly adopted to synthesize the lithium titanate with a lithium source, and finally the generated lithium titanate has larger particle size and poor performance.
CN 109888272 a discloses a preparation method of a low-cost lithium titanate material, which comprises the following steps: (1) reacting industrial metatitanic acid with hydrogen peroxide, and adding a proper amount of ammonia water to form a stable peroxotitanium complex solution; (2) and (2) weighing a lithium source according to a ratio, adding the lithium source into the titanium peroxide complex solution prepared in the step (1), adding a dispersing agent, stirring to form a uniform solution, drying, and roasting to obtain the titanic acid anxiety material. Firstly, the steps of separating solid and liquid materials, washing and the like are not carried out in the whole synthesis process, and impurities brought in by raw materials are completely retained in the product, so that the quality and the performance of the product are influenced; secondly, the solution phase of the material is directly dried and calcined, so that the material is easy to harden and agglomerate, which not only brings difficulty to the post-treatment of the process, but also can seriously affect the quality and performance of the product.
CN 110092413A discloses a method for preparing lithium titanate by a spray drying-solid phase method, wherein the method for preparing lithium titanate comprises the following steps: (1) weighing a titanium source, adding ammonia water, preparing industrial metatitanic acid under a first reaction condition, adding concentrated nitric acid, and performing ultrasonic treatment to obtain a titanyl nitrate clear solution; (2) weighing a lithium source, adding a dispersing agent and deionized water, and stirring to prepare a first solution; (3) mixing the titanyl nitrate clear solution with the first solution, and then drying by using a spray dryer to obtain precursor powder; (4) and roasting and cooling the precursor powder to prepare the lithium titanate. The method for synthesizing lithium titanate has two main defects, firstly, the steps of separating and washing solid and liquid materials are not needed in the synthesis process, and the nitric acid and other impurities as raw materials are completely retained in the product, so that the quality and the performance of the product are influenced; secondly, the nitric acid used for dissolving titanium has strong corrosivity, is directly used for spray drying without corresponding treatment in the preparation process, has great harm to spray equipment and is only in great potential safety hazard.
Disclosure of Invention
The synthesis of spinel lithium titanate in the prior art is generally divided into a solid-phase method and a liquid-phase method, the solid-phase method synthesis has low requirements on raw materials, but has the defects of long high-temperature calcination time, serious agglomeration of products after sintering and poor performance. The liquid phase method has the disadvantages of low calcination strength, small product particle size and good product performance, but has high requirements on titanium raw materials and is difficult to produce in large batch.
Aiming at the defects in the prior art, the invention provides a method for preparing high-purity nano lithium titanate by taking industrial metatitanic acid as a raw material, which has the advantages of low requirement on the raw material, small product particle size, good product performance and the like.
The invention relates to a method for preparing high-purity nano lithium titanate by using industrial metatitanic acid, which comprises the following steps:
A. mixing industrial metatitanic acid, hydrogen peroxide and ammonia water, and reacting at 0-5 ℃ to obtain a mixed solution;
B. heating the mixed solution, dropwise adding a lithium source and a dispersing agent into the mixed solution, heating to 60-80 ℃, and keeping the temperature;
C. and after the heat preservation is finished, separating, washing, drying and calcining the solid to obtain the high-purity nano lithium titanate.
Specifically, in the step a of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the mixing is to add the industrial metatitanic acid into a mixed solution of hydrogen peroxide and ammonia water.
Specifically, in the step a of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the industrial metatitanic acid is obtained after secondary washing.
Specifically, in the step a of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the amount of hydrogen peroxide is controlled to be more than 5 times of titanium, and the amount of ammonia water is controlled to be more than 2 times of titanium.
Further, in the step A of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the molar ratio of the industrial metatitanic acid to the hydrogen peroxide to the ammonia water is n (Ti) to N (NH) 3 ·H 2 O)﹕n(H 2 O 2 )＝1﹕2～4﹕5～10。
Furthermore, in the step A of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the molar ratio of the industrial metatitanic acid to the hydrogen peroxide to the ammonia water is n (Ti) to N (NH) 3 ·H 2 O)﹕n(H 2 O 2 )＝1﹕3～4﹕7～10。
Specifically, in the step A of the method for preparing the high-purity nano lithium titanate from the industrial metatitanic acid, the reaction time is 1-2 hours.
Preferably, in the step a of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the mass concentration of hydrogen peroxide is 10-30%. The mass concentration of the ammonia water is 10-20%.
Specifically, in step B of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the lithium source is at least one of lithium nitrate or lithium hydroxide.
Further, in the step B of the method for preparing high-purity nano lithium titanate by using industrial metatitanic acid, the concentration of the lithium source is 0.1-2 mol/L.
Specifically, in the step B of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the addition amount of the lithium source is n (li) n (ti) (0.85-0.95).
Specifically, in the step B of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the heat preservation time is calculated by taking the end of temperature rise or the end of lithium source dropping as a starting point, and the heat preservation time is 2-3 hours.
Preferably, in the step B of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the temperature rise is controlled and the lithium source is dropped.
Preferably, in the step B of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the temperature rise and the dropping of the lithium source are controlled to be synchronously finished.
Specifically, in the step B of the method for preparing high-purity nano lithium titanate from industrial metatitanic acid, the heating rate is less than 3 ℃/min. Preferably 2 to 3 ℃/min.
Specifically, in the step B of the method for preparing high-purity nano lithium titanate from the industrial metatitanic acid raw material, the dispersant is nonylphenol polyoxyethylene ether.
Preferably, in the step B of the method for preparing high-purity nano lithium titanate from the industrial metatitanic acid raw material, the addition amount of the dispersant is 1-2% of the total volume of the mixed solution and the lithium source.
Specifically, in the step C of the method for preparing high-purity nano lithium titanate from the industrial metatitanic acid raw material, the drying is spray drying.
Specifically, in the step C of the method for preparing high-purity nano lithium titanate from the industrial metatitanic acid raw material, the calcination temperature is 650-750 ℃. The time is 2-5 h.
Preferably, in the step C of the method for preparing high-purity nano lithium titanate from the industrial metatitanic acid raw material, the calcination temperature is 700-750 ℃. The time is 3-5 h.
The method has low requirement on the titanium raw material, only needs the common industrial metatitanic acid, does not need high-purity nano-scale titanium dioxide or high-valence organic titanium raw material, and has low raw material cost; the method has the advantages of simple preparation conditions, easy operation and low energy consumption. The product prepared by the method is the nano spinel lithium titanate, the impurity content is extremely low, the purity is extremely high, the comprehensive performance of the product is good, the 0.1C capacity is more than 170mAh/g, the 5C capacity is more than 160mAh/g, the particle size of the product is small, and the particle size of primary particles is about 20-50 nm.
In the method, the precursor of lithium metatitanate generated by hydrolysis has excellent reaction activity, the calcination strength adopted in the calcination process stage is obviously lower than that required by the synthesis of lithium titanate by the conventional solid phase method, the average calcination temperature is reduced by about 100 ℃, and the calcination time is reduced by more than about 8 hours. In the method, in the processes of material dissolution, hydrolysis, precipitation, filtration and washing, the impurities such as sulfate radicals, iron, magnesium, calcium, sodium, potassium and the like brought by the industrial metatitanic acid raw material are removed, and the obtained lithium titanate product has extremely low impurity content, extremely high purity and excellent performance.
Drawings
FIG. 1 XRD pattern of product of example 1
FIG. 2 SEM photograph of product of example 1
Detailed Description
The invention discloses a method for preparing a high-purity nano lithium titanate material by taking industrial metatitanic acid as a raw material, which comprises the following steps:
a. complete dissolution of the titanium source: under the condition of magnetic stirring in an ice-water bath at the temperature of 0-5 ℃, slowly adding industrial metatitanic acid into a mixed solution of hydrogen peroxide and ammonia water, and keeping the ice-water bath for 1-2 hours to obtain a clear yellow-green solution;
b. hydrolysis synthesis reaction: heating and heating the solution to clarify the yellow-green solution under the condition of stirring, dropwise adding a lithium source into the yellow-green solution at a constant speed according to the ratio of n (li) to n (Ti) to 0.85-0.95, adding a dispersant nonylphenol polyoxyethylene ether (NP-10) with the total volume of the solution being 1-2%, heating to 60-80 ℃, and preserving heat to obtain a white precipitate mixed solution;
c. filtering, washing, drying and calcining: and carrying out suction filtration on the white precipitate mixed solution to obtain a white precipitate, repeatedly washing the precipitate with deionized water, finally adding a small amount of deionized water for pulping, drying and granulating by using a spray dryer, and finally calcining the spray-dried material to obtain the high-purity nano lithium titanate material.
In the method, because the raw material metatitanic acid is difficult to react with the lithium source, and the metatitanic acid has strong adsorbability, the metatitanic acid can adsorb impurities such as sulfate radicals, iron, magnesium, calcium, sodium, potassium and the like in the working procedure, and the impurity content is high. In the step a of the method, the industrial metatitanic acid is added into the mixed solution of hydrogen peroxide and ammonia water for reaction to generate the ammonium peroxotitanate, so that the activity is improved, and the ammonium peroxotitanate can not adsorb impurities, thereby achieving the aim of removing impurities. In order to ensure that the titanium source is completely dissolved, sufficient hydrogen peroxide and ammonia water are needed, the amount of hydrogen peroxide is controlled to be more than 5 times of titanium, and the amount of ammonia water is controlled to be more than 2 times of titanium. Preferably, the molar ratio of metatitanic acid to hydrogen peroxide to ammonia water is controlled to N (NH), (Ti) to N (NH) 3 ·H 2 O)﹕n(H 2 O 2 ) The ratio of the length to the length is 1: 2 to 4: 5 to 10. Further, the molar ratio n (Ti) to N (NH) of metatitanic acid, hydrogen peroxide and aqueous ammonia was controlled 3 ·H 2 O)﹕n(H 2 O 2 )＝1﹕3～4﹕7～10。
In the method, by utilizing the characteristics of strong reaction activity of hydrogen peroxide, easily controlled concentration and no impurity, and adopting a mode of slowly heating and slowly dripping a lithium source, on one hand, the ammonium peroxotitanate is hydrolyzed by heating and decomposing the hydrogen peroxide, and on the other hand, the titanium lithium is co-hydrolyzed by adding the lithium source to generate the lithium metatitanate precursor with excellent activity.
The ammonium peroxotitanate hydrolyzes to form metatitanic acid in the heating process, has adsorption capacity, and in order to ensure the product quality, a lithium source exists when metatitanic acid is generated by hydrolysis, so that the metatitanic acid is prevented from adsorbing impurities in a solution, and the product purity is reduced. Preferably, the dropping of the lithium source is started while controlling the heating to be started. Preferably, the dropping of the lithium source is completed at the same time as the completion of the temperature increase. In order to ensure the full reaction of the lithium metatitanate precursor, the full utilization of lithium ions, the product stabilization and the like, the heat preservation is needed for 2-3 hours.
Meanwhile, during the hydrolysis synthesis reaction, time is wasted due to too low temperature rise speed, too high temperature rise speed causes too high solution hydrolysis reaction speed, and the particle size of the generated lithium metatitanate precursor is too large, so that the product performance is reduced. Preferably, the rate of temperature rise is less than 3 ℃ per minute. Preferably, the temperature is controlled to be 2-3 ℃/min. The highest temperature is controlled within 80 ℃, and if the temperature is too high, the reaction is violent, and the particle size of the product is larger. Preferably, the temperature is controlled to be 60-80 ℃. More preferably, the temperature is controlled to be 70-80 ℃.
In the method, the dispersing agent is added to reduce aggregation of hydrolysate particles in a solution system, reduce product aggregation, promote the reaction of lithium metatitanate precursors and reduce the final particle size of products. Nonylphenol polyoxyethylene ether (NP-10) is preferred as the dispersant of the present invention in order to carry no impurities.
In the method, the precursor of lithium metatitanate generated by hydrolysis has excellent reaction activity, the calcination strength adopted in the calcination process stage is obviously lower than that required by the synthesis of lithium titanate by the conventional solid phase method, the average calcination temperature is reduced by about 100 ℃, and the calcination time is reduced by more than about 8 hours. And in the final calcining process, the calcining is controlled at 650-750 ℃ for 2-5 h, the temperature is lower than 650 ℃, the calcining reaction is insufficient, energy is wasted when the temperature is higher than 750 ℃, and the agglomeration phenomenon also exists in the materials, so that the product performance is influenced. The calcination temperature is preferably 700 to 750 ℃. Calcining for 3-5 h.
In the method, in the processes of material dissolution, hydrolysis, precipitation, filtration and washing, the impurities such as sulfate radicals, iron, magnesium, calcium, sodium, potassium and the like brought by the industrial metatitanic acid raw material are removed, and the obtained lithium titanate product has extremely low impurity content, extremely high purity and excellent performance.
Example 1
(1) Weighing a batch of 10 kg of industrial metatitanic acid (a product produced by the normal source science and technology in Panzhihua city and washed by water for the second time), drying at low temperature, and measuring the titanium content for later use.
(2) Taking 200g of dried metatitanic acid, and mixing n (Ti) N (NH) 3 ·H 2 O)﹕n(H 2 O 2 ) Preparing a mixed solution of ammonia water and hydrogen peroxide, wherein the concentration of the hydrogen peroxide is 30% and the concentration of the ammonia water is 20%, slowly adding the dried industrial metatitanic acid into the mixed solution, keeping an ice-water bath, and stirring for reaction for 2 hours to obtain clear bright yellow ammonium peroxotitanate (NH) 4 TiO 3 ·H 2 O 2 ) And (3) solution.
(3) Preparing a 1mol/L lithium hydroxide solution in advance according to the ratio of n (li) to n (Ti) being 0.95, slowly dropping the solution into the yellow solution obtained in the step 2 by using a dropping funnel, rapidly stirring the yellow titanium solution while dropping the lithium solution, heating the solution in a water bath at a controlled temperature rise rate of 2 ℃/min to 80 ℃, adding NP-10 accounting for 1% of the total amount of the solution as a dispersing agent, and keeping the temperature for 1 hour to obtain a white precipitate mixed solution.
(4) And 3, filtering the solution in the step 3 under reduced pressure to obtain white precipitate, washing the white precipitate with deionized water for three times, adding deionized water into a filter cake for pulping, spray-drying the slurry to obtain white powder, and calcining the white powder in a box-type furnace at the calcining temperature of 750 ℃ for 3 hours to obtain the final spinel lithium titanate product, wherein the XRD test of the product is shown in figure 1, and the SEM test is shown in figure 2. According to SEM, after spray granulation, the product forms porous micron-sized secondary particles, the primary particles are nano-sized, a half-cell test is shown in table 1, the performance is in an excellent level relative to similar products, the main content and the impurity content are shown in table 2, the impurity content is far lower than the requirements of national standard YST 825-.
Table 1 example 1 half-cell charge and discharge performance testing of the product
Figure BDA0002513199960000051
Table 2 example 1 product element content testing
Figure BDA0002513199960000052
Figure BDA0002513199960000061
Example 2
(1) Weighing a batch of 10 kg of industrial metatitanic acid (a product produced by the normal source science and technology in Panzhihua city and washed by water for the second time), drying at low temperature, and measuring the titanium content for later use.
(2) Taking 200g of dried metatitanic acid, and mixing n (Ti) N (NH) 3 ·H 2 O)﹕n(H 2 O 2 ) Preparing a mixed solution of ammonia water and hydrogen peroxide, wherein the concentration of the hydrogen peroxide is 20% and the concentration of the ammonia water is 20%, slowly adding the dried industrial metatitanic acid into the mixed solution, keeping an ice-water bath, and stirring for reaction for 2 hours to obtain clear bright yellow ammonium peroxotitanate (NH) 4 TiO 3 ·H 2 O 2 ) And (3) solution.
(3) A0.5 mol/L lithium hydroxide solution was prepared in advance, and the solution was slowly dropped into the yellow solution obtained in the step 2 using a dropping funnel while rapidly stirring the yellow titanium solution, and the mixed solution was heated in a water bath at a temperature rising rate of 2 ℃/min to 70 ℃, and NP-10 in an amount of 1% of the total amount of the solution was added as a dispersant, and the mixture was kept warm for 2 hours to obtain a white precipitate mixed solution.
(4) And (3) filtering the solution obtained in the step (3) under reduced pressure to obtain a white precipitate, washing the white precipitate with deionized water for three times, adding deionized water into a filter cake for pulping, spray-drying the slurry to obtain white powder, and calcining the white powder in a box-type furnace at 700 ℃ for 4 hours to obtain a final spinel lithium titanate product, wherein the product test result is similar to that in example 1.
Example 3
(1) Weighing a batch of 10 kg of industrial metatitanic acid (a product produced by the normal source science and technology in Panzhihua city and washed by water for the second time), drying at low temperature, and measuring the titanium content for later use.
(2) Taking 200g of dried metatitanic acid, and mixing n (Ti) N (NH) 3 ·H 2 O)﹕n(H 2 O 2 ) Preparing a mixed solution of ammonia water and hydrogen peroxide, wherein the concentration of the hydrogen peroxide is 30% and the concentration of the ammonia water is 15%, slowly adding the dried industrial metatitanic acid into the mixed solution, keeping an ice-water bath, and stirring for reaction for 2 hours to obtain clear bright yellow ammonium peroxotitanate (NH) 4 TiO 3 ·H 2 O 2 ) And (3) solution.
(3) A0.5 mol/L lithium hydroxide solution was prepared in advance, and the solution was slowly dropped into the yellow solution obtained in the 2 steps using a dropping funnel while rapidly stirring the yellow titanium solution, and the solution was heated in a water bath at a controlled rate of 3 ℃/min to 80 ℃, followed by addition of NP-10 as a dispersant in an amount of 1% of the total amount of the solution and heat preservation for 2 hours to obtain a white precipitate mixed solution.
(4) And 3, filtering the solution in the step 1 under reduced pressure to obtain white precipitate, washing the white precipitate for three times by using deionized water, adding the deionized water into a filter cake for pulping, spray-drying the slurry to obtain white powder, and calcining the white powder in a box-type furnace at the calcining temperature of 650 ℃ for 5 hours to obtain the final spinel lithium titanate product, wherein the product test result is similar to that in the example 1.
Comparative example 1
(1) Weighing a batch of 10 kg of industrial metatitanic acid (a product produced by the normal source science and technology in Panzhihua city and washed by water for the second time), drying at low temperature, and measuring the titanium content for later use.
(2) Taking 200g of dried metatitanic acid powder as n (Ti) N (NH) 3 ·H 2 O)﹕n(H 2 O 2 ) Preparing a mixed solution of ammonia water and hydrogen peroxide at a concentration of 30%The ammonia water concentration is 20 percent, the dried industrial metatitanic acid is slowly added into the mixed solution, the mixed solution is kept in an ice water bath to be stirred and react for 2 hours, and the clear bright yellow ammonium peroxotitanate (NH) is obtained 4 TiO 3 ·H 2 O 2 ) And (3) solution.
(3) A1 mol/L lithium hydroxide solution was prepared in advance as n (li): n (Ti) ═ 0.95, and the solution was slowly dropped into the yellow solution obtained in the 2 steps using a dropping funnel, followed by addition of NP-10 as a dispersant in an amount of 1% of the total amount of the solution and aging for 1 hour to obtain a pale yellow solution.
(4) And (3) directly drying the mixed solution obtained in the step (3) by using a spray dryer to obtain precursor powder, and then putting the white powder into a box-type furnace for calcination at the temperature of 650 ℃ for 5 hours to obtain the final spinel lithium titanate product. The comparison of the impurity content of the tested product with the examples is shown in Table 3, the impurity content is far higher than that of examples 1, 2 and 3, and is similar to that of the industrial metatitanic acid raw material, which indicates that the impurities are brought by the industrial metatitanic acid and do not meet the impurity content requirement of the national standard YST 825-.
Table 3 elemental content testing of comparative example 1 product
Figure BDA0002513199960000071

Claims (5)

1. The method for preparing high-purity nano lithium titanate by using industrial metatitanic acid is characterized by comprising the following steps of: the method comprises the following steps:
A. mixing industrial metatitanic acid, hydrogen peroxide and ammonia water, reacting for 1-2 hours at 0-5 ℃ to obtain a mixed solution, controlling the amount of hydrogen peroxide to be more than 5 times that of titanium, controlling the amount of ammonia water to be more than 2 times that of titanium, controlling the mass concentration of hydrogen peroxide to be 10-30%, controlling the mass concentration of ammonia water to be 10-20%, and controlling the molar ratio n (Ti) N (NH) of industrial metatitanic acid to ammonia water to hydrogen peroxide 3 ·H 2 O)﹕n(H 2 O 2 ) =1﹕2～4﹕5～10；
B. Heating the mixed liquid, dropwise adding a lithium source and a dispersing agent into the mixed liquid, wherein the lithium source is at least one of lithium nitrate or lithium hydroxide, the dispersing agent is nonylphenol polyoxyethylene ether, the concentration of the lithium source is 0.1-2 mol/L, the addition amount of the lithium source is n (Li) n (Ti) = 0.85-0.95, the addition amount of the dispersing agent is 1-2% of the total volume of the mixed liquid and the lithium source, heating to 60-80 ℃ and preserving heat, calculating the heat preservation time by taking the end of heating or the end of dropwise adding the lithium source as a starting point, and keeping the heat preservation time for 2-3 hours, wherein the heating and the dropwise adding of the lithium source are started synchronously;
C. and after the heat preservation is finished, separating, washing, drying and calcining the solid, wherein the calcining temperature is 650-750 ℃, and the calcining time is 2-5 hours, so that the high-purity nano lithium titanate is obtained.
2. The method for preparing high-purity nano lithium titanate from industrial metatitanic acid according to claim 1, wherein the method comprises the following steps: and in the step B, finishing the temperature rise and the dropwise adding of the lithium source synchronously.
3. The method for preparing high-purity nano lithium titanate from industrial metatitanic acid according to any one of claims 1 to 2, wherein the method comprises the following steps: in the step B, the heating rate is less than 3 ℃/min.
4. The method for preparing high-purity nano lithium titanate from industrial metatitanic acid according to any one of claims 1 to 2, wherein the method comprises the following steps: in the step B, the heating rate is 2-3 ℃/min.
5. The method for preparing high-purity nano lithium titanate from industrial metatitanic acid according to any one of claims 1 to 2, wherein the method comprises the following steps: in step C, the drying is spray drying.
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