CN102820459A - Preparation method for lithium titanate material with high specific energy from mesoporous titanium dioxide - Google Patents
Preparation method for lithium titanate material with high specific energy from mesoporous titanium dioxide Download PDFInfo
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- CN102820459A CN102820459A CN2012102535774A CN201210253577A CN102820459A CN 102820459 A CN102820459 A CN 102820459A CN 2012102535774 A CN2012102535774 A CN 2012102535774A CN 201210253577 A CN201210253577 A CN 201210253577A CN 102820459 A CN102820459 A CN 102820459A
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method for a lithium titanate material with high specific energy from mesoporous titanium dioxide, which belongs to the fields of preparation technologies for electrode materials and energy. The preparation method provided by the invention comprises the following steps: (1) preparation of mesoporous titanium dioxide: a step of preparing nanometer mesoporous titanium dioxide by using a template precipitation method and heat treatment; (2) material mixing: a step of uniformly mixing nanometer mesoporous titanium dioxide, a lithium salt and a binder in a ball mill according to a certain mol ratio so as to obtain wet precursor slurry; (3) composite granulation: a step of transferring the wet precursor slurry into a vacuum rotary dryer for drying and shaping of a material so as to obtain precursor powder; and (4) calcination: a step of calcining the precursor powder in a tubular furnace in an inert atmosphere so as to prepare mesoporous lithium titanate with high specific energy. The lithium titanate material prepared in the invention has the advantages of good stability, high tap density, high electronic conductivity, excellent electrochemical performance, etc., and is suitable for industrial production.
Description
Technical field
The present invention relates to lithium ion battery negative material, the preparation method of the synthetic high specific energy lithium titanate material of particularly a kind of mesoporous TiO 2 belongs to the electrochemical material field.
Background technology
At present; Commercial lithium ion battery negative material mainly is the graphite-like material with carbon element; Said material has bigger specific capacity, but the major defect that exists is: with the electrolyte formation surface passivated membrane that reacts, cause electrolyte consumption and coulomb efficient is lower first; Separate out Li dendrite, make battery short circuit, bring serious potential safety hazard.Spinel type lithium titanate (Li
4Ti
5O
12) having remarkable advantages as lithium ion battery negative material: current potential is high, does not react with electrolyte commonly used, and security performance is good; Be a kind of zero strain electrode material, lithium ion embeds therein and to deviate from caused change in volume very little, long service life; Higher chemical diffusion coefficient (2 * 10 is arranged
-8Cm
2/ s), lithium ion has migration rate faster therein, is fit to fast charging and discharging.While Li
4Ti
5O
12Also have characteristics such as anti-over-charging and Heat stability is good.But Li
4Ti
5O
12The subject matter that exists is that ion electronic conductivity difference and tap density are low.When under the high magnification environment, working, Li
4Ti
5O
12Specific capacity decay rapidly, and the field of especially attracting attention for the practical application of lithium ion battery in this whole world of electrokinetic cell, the high magnification operating characteristic of lithium ion battery be decision its can obtain one of key factor of commercial applications; Low tap density must cause low specific energy, and its application in various compact powers is fettered, and is unfavorable for equally commercially producing.
Summary of the invention
The objective of the invention is in order to overcome the deficiency of above-mentioned prior art, the preparation method of the synthetic high specific energy lithium titanate material of a kind of mesoporous TiO 2 is provided.Prepared the mesoporous lithium titanate of high specific energy with high conduction performance and tap density through synthesis of nano mesoporous TiO 2 and compound granulating technique.
The present invention adopts following technical scheme to achieve these goals:
The preparation method of the synthetic mesoporous lithium titanate material of high specific energy of a kind of mesoporous TiO 2 specifically comprises following preparation process:
(1) preparation mesoporous TiO 2: the sodium carbonate liquor and the mass percent that in container, add concentration and be 40-60% are the template solution of 1-5% and stir; The volume ratio of sodium carbonate liquor and template solution is 10:1-5:1; Drip the titanyl sulfate solution that concentration is 120-160g/L then; Stop during for 6.5-7.0 to the pH value, filter after ageing 2-6 hour and obtain TiO 2 precursor; Use again till absolute ethanol washing sediment to the sulfate radical-free, place oven dry in baking oven 2-6 hour after, place Muffle furnace again, 450-650 ℃ of down calcining 1-3 hour, be cooled to room temperature and promptly get sharp ore deposit titanium type nanometer mesoporous TiO 2 powder;
(2) batch mixing: in the Li:Ti mol ratio is that the ratio of 0.80-0.86 takes by weighing lithium salts and titanium dioxide in ball mill container; With the organic solvent is dispersant; Add adhesive solution, wherein adhesive accounted for the 1-15% of material gross mass, with the rotating speed ball milling of 400r/min 4-12 hour; Fully mix, make the presoma wet slurry;
(3) compound granulation: the presoma wet slurry of gained is shifted in the supplies room of vacuum rotary dryer into, be heated to 60-100 ℃, start vacuum extractor simultaneously, the rotary speed of setting material is 1-30r/min, until the dry materials moulding;
(4) calcining: dried material is placed tube furnace, and the heating rate with 2-10 ℃/min under inert gas is heated to 750-950 ℃, and insulation 8-24h is cooled to room temperature, promptly gets the mesoporous lithium titanate of high specific energy after the pulverizing.
Template in the said step (1) is a kind of of non-ionic surface active agent polyethylene glycol, P123.
Template in the said step (1) is a kind of in non-surface-active agent glycerine, the pentaerythrite.
Lithium salts in the said step (2) is a kind of in lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium chloride, the lithium fluoride.
Titanium dioxide in the said step (2) is homemade sharp ore deposit titanium type nano meso-porous titanium dioxide.
Organic solvent in the said step (2) is one or more mixed solvents in methyl alcohol, ethanol, the acetone.
Adhesive in the said step (2) is that in sugar, starch, polyethylene glycol, polyvinyl butyral resin (PVB), the phenolic resins one or more are combined.
Dissolution mechanism during adhesive formulations prepared from solutions in the said step (2) is: to the container that fills absolute ethyl alcohol or deionized water and be under the stirring condition, slowly add should be able to dissolve mutually adhesive.
Beneficial effect of the present invention:
(1) adopting inorganic titanium salt and inorganic salts precipitation reagent is primary raw material, and water is that medium is prepared nano meso-porous titanium dioxide, through regulating template kind and concentration and calcining intensity etc., can obtain the mesoporous TiO 2 powder of different apertures, different specific areas.
(2) the present invention is with self-control mesoporous nano TiO
2The lithium ionic cell cathode material lithium titanate of preparing for the titanium source has the mesoporous nano structure; Improved the specific area of lithium titanate greatly; Thereby reduce the diffusion length of lithium ion in lithium titanate; Help improving the storage lithium specific capacity of lithium titanate, help the infiltration of electrolyte simultaneously, thereby improve the electronic conductivity of lithium titanate anode material.
(3) the present invention has used the compound granulating technique of a kind of rotary evaporation, makes the moulding of presoma wet slurry primary drying, and is prepared into form of spherical particles, has strengthened the bonding tightness of each component of presintering material, and has improved the tap density of material behind the sintering.
(4) lithium titanate anode material that makes of this method, its tap density can reach 1.0-1.2g/cm
3, the 0.2C specific discharge capacity can reach 168-172mAh/g under the normal temperature, and the 2C discharge can reach 165-170 mAh/g.
Description of drawings
Fig. 1 is the TEM figure of nano meso-porous titanium dioxide material;
Fig. 2 is the first charge-discharge curve chart under the mesoporous lithium titanate material 0.2C of high specific energy.
Embodiment
Below in conjunction with embodiment the present invention is done further description:
Embodiment 1:
(1) preparation mesoporous TiO 2: in container, adding concentration is that 50% sodium carbonate liquor 50mL and mass percent are 5% surfactant polyethylene solution 5mL and stir; Slowly dripping concentration is the titanyl sulfate solution of 130g/L; To the pH value is to stop in 7.0 o'clock, and ageing was filtered after 3 hours; Till absolute ethanol washing sediment to sulfate radical-free, place 80 ℃ of baking ovens after 3 hours product, change in the Muffle furnace, be warming up to 450 ℃ and be incubated 1.5 hours with the speed of 5 ℃/min, grind after being cooled to room temperature, promptly obtaining specific area is 150m
2About/g, pore-size distribution is the sharp ore deposit titanium type nanometer mesoporous TiO 2 powder of 10-15nm;
(2) batch mixing: the ratio in Li:Ti mol ratio 0.84 takes by weighing lithium salts and self-control mesoporous TiO 2; In ball mill container with absolute ethyl alcohol as solvent; And adding adhesive glucose/deionized water solution; Wherein glucose accounts for 5% of material gross mass, with the rotating speed ball milling of 400r/min 6 hours, makes the presoma wet slurry;
(3) compound granulation: the presoma wet slurry of gained is shifted in the supplies room of vacuum rotary dryer into; Be heated to 80 ℃; Start vacuum extractor simultaneously, the rotary speed of setting material is 5r/min, vacuumize 10 hours; The presoma material that obtains is the high-density balls shape, and particle diameter is 3-5cm;
(4) calcining: the dried material of step 3 is placed tube furnace, and the heating rate with 5 ℃/min under nitrogen atmosphere is heated to 800 ℃, and insulation 14h is cooled to room temperature, promptly gets the mesoporous lithium titanate of high specific energy after the grinding.
Embodiment 2:
(1) preparation mesoporous TiO 2: in container, adding concentration is that 50% sodium carbonate sodium solution 50mL and mass percent are 3% surfactant polyethylene solution 5mL and stir; Slowly dripping concentration is the titanyl sulfate solution of 130g/L; To the pH value is to stop in 7.0 o'clock, and ageing was filtered after 3 hours; Till absolute ethanol washing sediment to sulfate radical-free, place 80 ℃ of baking ovens after 3 hours product, change in the Muffle furnace, be warming up to 500 ℃ and be incubated 2 hours with the speed of 5 ℃/min, grind after being cooled to room temperature, promptly obtaining specific area is 100m
2About/g, pore-size distribution is the sharp ore deposit titanium type nanometer mesoporous TiO 2 powder of 5-10nm;
(2) batch mixing: the ratio of Li:Ti=0.85 takes by weighing lithium salts and self-control mesoporous TiO 2 in molar ratio; In ball mill container with absolute ethyl alcohol as solvent; And adding adhesive glucose/deionized water solution; Wherein glucose accounts for 3% of material gross mass, with the rotating speed ball milling of 400r/min 6 hours, makes the presoma wet slurry;
(3) compound granulation: the presoma wet slurry of gained is shifted in the supplies room of vacuum rotary dryer into; Be heated to 80 ℃; Start vacuum extractor simultaneously, the rotary speed of setting material is 5r/min, vacuumize 10 hours; The presoma material that obtains is the high-density balls shape, and particle diameter is 2-4cm;
(4) the dried material of step 3 is placed tube furnace, the heating rate with 5 ℃/min under nitrogen atmosphere is heated to 850 ℃, and insulation 14h is cooled to room temperature, promptly gets the mesoporous lithium titanate of high specific energy after the grinding.
Embodiment 3:
(1) preparation mesoporous TiO 2: in container, adding concentration is that 50% sodium carbonate liquor 50mL and mass percent are 5% surfactant polyethylene solution 5mL and stir; Slowly dripping concentration is the titanyl sulfate solution of 130g/L; To the pH value is to stop in 6.5 o'clock, and ageing was filtered after 3 hours; With with till absolute ethanol washing sediment to the sulfate radical-free, place 80 ℃ of baking ovens after 3 hours product, change in the Muffle furnace, be warming up to 550 ℃ and be incubated 1.0 hours with the speed of 5 ℃/min, grind after being cooled to room temperature, promptly obtaining specific area is 150m
2About/g, pore-size distribution is the sharp ore deposit titanium type nanometer mesoporous TiO 2 powder of 10-15nm;
(2) batch mixing: the ratio of Li:Ti=0.83 takes by weighing lithium salts and self-control mesoporous TiO 2 in molar ratio; In ball mill container with absolute ethyl alcohol as solvent; And adding adhesive glucose/deionized water solution; Wherein glucose accounts for 3% of material gross mass, with the rotating speed ball milling of 400r/min 6 hours, makes the presoma wet slurry;
(3) compound granulation: the presoma wet slurry of gained is shifted in the supplies room of vacuum rotary dryer into; Be heated to 80 ℃; Start vacuum extractor simultaneously, the rotary speed of setting material is 10r/min, vacuumize 10 hours; The presoma material that obtains is the high-density balls shape, and particle diameter is 1-1.5cm;
(4) calcining: the dried material of step 3 is placed tube furnace, and the heating rate with 5 ℃/min under nitrogen atmosphere is heated to 800 ℃, and insulation 12h is cooled to room temperature, promptly gets the mesoporous lithium titanate of high specific energy after the grinding.
Embodiment 4:
(1) preparation mesoporous TiO 2: in container, adding concentration is that 50% sodium carbonate liquor 50mL and mass percent are 3% surfactant polyethylene solution 5mL and stir; Slowly dripping concentration is the titanyl sulfate solution of 130g/L; To the pH value is to stop in 6.5 o'clock, and ageing was filtered after 3 hours; Till absolute ethanol washing sediment to sulfate radical-free, place 80 ℃ of baking ovens after 3 hours product, change in the Muffle furnace, be warming up to 600 ℃ and be incubated 1.5 hours with the speed of 5 ℃/min, grind after being cooled to room temperature, promptly obtaining specific area is 100m
2About/g, pore-size distribution is the sharp ore deposit titanium type nanometer mesoporous TiO 2 powder of 5-10nm;
(2) batch mixing: the ratio of Li:Ti=0.83 takes by weighing lithium salts and self-control mesoporous TiO 2 in molar ratio; In ball mill container with absolute ethyl alcohol as solvent; And adding adhesive glucose/deionized water solution; Wherein glucose accounts for 5% of material gross mass, with the rotating speed ball milling of 400r/min 6 hours, makes the presoma wet slurry;
(3) compound granulation: the presoma wet slurry of gained is shifted in the supplies room of vacuum rotary dryer into; Be heated to 80 ℃; Start vacuum extractor simultaneously, the rotary speed of setting material is 10r/min, vacuumize 10 hours; The presoma material that obtains is the high-density balls shape, and particle diameter is 1-2cm;
(4) calcining: the dried material of step 3 is placed tube furnace, and the heating rate with 5 ℃/min under nitrogen atmosphere is heated to 850 ℃, and insulation 12h is cooled to room temperature, promptly gets the mesoporous lithium titanate of high specific energy after the grinding.
Claims (8)
1. the preparation method of the synthetic high specific energy lithium titanate material of a mesoporous TiO 2 is characterized in that comprising following preparation process:
(1) preparation mesoporous TiO 2: the sodium carbonate liquor and the mass percent that in container, add concentration and be 40-60% are the template solution of 1-5% and stir; The volume ratio of sodium carbonate liquor and template solution is 10:1-5:1; Drip the titanyl sulfate solution that concentration is 120-160g/L then; Stop during for 6.5-7.0 to the pH value, filter after ageing 2-6 hour and obtain TiO 2 precursor; Use again till absolute ethanol washing sediment to the sulfate radical-free, place oven dry in baking oven 2-6 hour after, place Muffle furnace again, 450-650 ℃ of down calcining 1-3 hour, be cooled to room temperature and promptly get sharp ore deposit titanium type nanometer mesoporous TiO 2 powder;
(2) batch mixing: in the Li:Ti mol ratio is that the ratio of 0.80-0.86 takes by weighing lithium salts and titanium dioxide in ball mill container; With the organic solvent is dispersant; Add adhesive solution, wherein adhesive accounted for the 1-15% of material gross mass, with the rotating speed ball milling of 400r/min 4-12 hour; Fully mix, make the presoma wet slurry;
(3) compound granulation: the presoma wet slurry of gained is shifted in the supplies room of vacuum rotary dryer into, be heated to 60-100 ℃, start vacuum extractor simultaneously, the rotary speed of setting material is 1-30r/min, until the dry materials moulding;
(4) calcining: dried material is placed tube furnace, and the heating rate with 2-10 ℃/min under inert gas is heated to 750-950 ℃, and insulation 8-24h is cooled to room temperature, promptly gets the mesoporous lithium titanate of high specific energy after the pulverizing.
2. the preparation method of the synthetic high specific energy lithium titanate material of mesoporous TiO 2 according to claim 1, it is characterized in that: the template described in the step (1) is a kind of of non-ionic surface active agent polyethylene glycol, P123.
3. the preparation method of the synthetic high specific energy lithium titanate material of mesoporous TiO 2 according to claim 1 is characterized in that: the described template of step (1) is a kind of in non-surface-active agent glycerine, the pentaerythrite.
4. the preparation method of the synthetic high specific energy lithium titanate material of mesoporous TiO 2 according to claim 1 is characterized in that: the described lithium salts of step (2) is a kind of in lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium chloride, the lithium fluoride.
5. the preparation method of the synthetic high specific energy lithium titanate material of mesoporous TiO 2 according to claim 1, it is characterized in that: the described titanium dioxide of step (2) is homemade sharp ore deposit titanium type nano meso-porous titanium dioxide.
6. the preparation method of the synthetic high specific energy lithium titanate material of mesoporous TiO 2 according to claim 1, it is characterized in that: the described organic solvent of step (2) is one or more mixed solvents in methyl alcohol, ethanol, the acetone.
7. the preparation method of the synthetic high specific energy lithium titanate material of mesoporous TiO 2 according to claim 1 is characterized in that: the described adhesive of step (2) is combined in sugar, starch, polyethylene glycol, polyvinyl butyral resin (PVB), the phenolic resins one or more.
8. the preparation method of the synthetic high specific energy lithium titanate material of mesoporous TiO 2 according to claim 1; It is characterized in that: the dissolution mechanism during the described adhesive formulations prepared from solutions of step (2) is: to the container that fills absolute ethyl alcohol or deionized water and be under the stirring condition, slowly add should be able to dissolve mutually adhesive.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104009236A (en) * | 2014-06-10 | 2014-08-27 | 华东理工大学 | Lithium titanate mesoporous single-crystal nanoparticle/reduced graphene oxide composite material as well as preparation method and application thereof |
| CN104600278A (en) * | 2014-12-31 | 2015-05-06 | 江苏江大环保科技开发有限公司 | Preparation method and application of graphene/lithium titanate composite material |
| CN104617273A (en) * | 2015-02-04 | 2015-05-13 | 安徽师范大学 | Spherical porous lithium titanate/titanium dioxide composite material as well as preparation method and application of composite material |
| CN105036182A (en) * | 2015-06-15 | 2015-11-11 | 山东玉皇新能源科技有限公司 | Preparation method and application of high-purity lithium titanate negative pole material |
| CN106972170A (en) * | 2017-05-27 | 2017-07-21 | 河北省科学院能源研究所 | A kind of lithium titanate electrode material with composite pore structural and preparation method thereof |
| CN107108256A (en) * | 2014-10-24 | 2017-08-29 | 大塚化学株式会社 | Porous titanate compound particle and its manufacture method |
| CN108946799A (en) * | 2018-09-26 | 2018-12-07 | 山东精工电子科技有限公司 | The method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate |
| CN113036121A (en) * | 2021-03-05 | 2021-06-25 | 大连理工大学 | Carbon-coated transition metal sulfide nanoflower structure, preparation method and application thereof |
| WO2022078015A1 (en) * | 2020-10-16 | 2022-04-21 | 安徽景成新材料有限公司 | Method for preparing titanium dioxide powder in different morphologies by using solid-phase process |
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| CN104009236A (en) * | 2014-06-10 | 2014-08-27 | 华东理工大学 | Lithium titanate mesoporous single-crystal nanoparticle/reduced graphene oxide composite material as well as preparation method and application thereof |
| CN107108256A (en) * | 2014-10-24 | 2017-08-29 | 大塚化学株式会社 | Porous titanate compound particle and its manufacture method |
| CN107108256B (en) * | 2014-10-24 | 2018-11-30 | 大塚化学株式会社 | porous titanate compound particle and its manufacturing method |
| CN104600278A (en) * | 2014-12-31 | 2015-05-06 | 江苏江大环保科技开发有限公司 | Preparation method and application of graphene/lithium titanate composite material |
| CN104617273A (en) * | 2015-02-04 | 2015-05-13 | 安徽师范大学 | Spherical porous lithium titanate/titanium dioxide composite material as well as preparation method and application of composite material |
| CN105036182A (en) * | 2015-06-15 | 2015-11-11 | 山东玉皇新能源科技有限公司 | Preparation method and application of high-purity lithium titanate negative pole material |
| CN105036182B (en) * | 2015-06-15 | 2017-03-08 | 山东玉皇新能源科技有限公司 | A kind of preparation method and applications of high-purity lithium titanate anode material |
| CN106972170A (en) * | 2017-05-27 | 2017-07-21 | 河北省科学院能源研究所 | A kind of lithium titanate electrode material with composite pore structural and preparation method thereof |
| CN108946799A (en) * | 2018-09-26 | 2018-12-07 | 山东精工电子科技有限公司 | The method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate |
| WO2022078015A1 (en) * | 2020-10-16 | 2022-04-21 | 安徽景成新材料有限公司 | Method for preparing titanium dioxide powder in different morphologies by using solid-phase process |
| CN113036121A (en) * | 2021-03-05 | 2021-06-25 | 大连理工大学 | Carbon-coated transition metal sulfide nanoflower structure, preparation method and application thereof |
| CN113036121B (en) * | 2021-03-05 | 2022-02-15 | 大连理工大学 | Carbon-coated transition metal sulfide nanoflower structure, preparation method and application thereof |
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Application publication date: 20121212 |