CN102820462A - Preparation process of anode material lithium manganate of spherical structure for lithium ion battery - Google Patents

Preparation process of anode material lithium manganate of spherical structure for lithium ion battery Download PDF

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Publication number
CN102820462A
CN102820462A CN2012103054894A CN201210305489A CN102820462A CN 102820462 A CN102820462 A CN 102820462A CN 2012103054894 A CN2012103054894 A CN 2012103054894A CN 201210305489 A CN201210305489 A CN 201210305489A CN 102820462 A CN102820462 A CN 102820462A
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lithium
spherical
anode material
manganese
solution
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王昌菊
孙卫华
孙朝军
李世辉
王艳红
王锡芬
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ANHUI ALAND NEW ENERGY MATERIALS Co Ltd
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ANHUI ALAND NEW ENERGY MATERIALS Co Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to the field of lithium ion battery materials, in particular to a preparation process of anode material lithium manganate (LiMn2O4) of a spherical structure for a lithium ion battery. Metal salt of manganese is used as a raw material and is dissolved into hot water to prepare solution of a certain concentration, the solution of the metal manganese and a precipitant simultaneously and concurrently flow into a reaction container according to a certain flow speed under a stirring condition; air is introduced to perform synthesis reaction; and spherical Mn3O4 precursor is obtained through aging and then is calcined with a lithium source to obtain the spherical anode material lithium manganate LiMn2O4 for the lithium ion battery. The preparation process of preparing the anode material lithium manganate LiMn2O4 of the lithium ion battery by taking the self-made spherical Mn3O4 as a precursor has the advantages of simple synthesis method, easiness in control over a process, high efficiency, low cost, energy and resource saving and suitability for industrial production.

Description

The preparation technology of spherical structure lithium cell anode material lithium manganate
Technical field
The present invention relates to the lithium ion battery material field, particularly a kind of spherical structure lithium cell anode material lithium manganate (LiMn 2O 4) preparation technology.
Background technology
The positive electrode that is used for lithium ion battery mainly contains LiCoO 2, LiNiO 2And LiMn 2O 4Though LiCoO 2Realized suitability for industrialized production, but its shortage of resources, cost an arm and a leg and toxic that these all become the unfavorable factor of restriction lithium ion battery industrial boom.Although LiNiO 2Become with its higher capacity and lower price and to be hopeful to substitute LiCoO 2One of positive electrode, but but difficulty relatively of its preparation, crystal structure is very responsive to the condition of preparation, is difficult to obtain stable material, thereby has limited its development.And spinelle LiMn 2O 4Not only on price, occupy very big advantage, and it is good to have a fail safe, non-environmental-pollution; Operating voltage is high; Characteristics such as with low cost, its three-dimensional tunnel structure more helps the embedding of lithium ion than lamellar compound and deviates from, so it is considered to be hopeful most to replace LiCoO 2One of positive electrode, and extremely researcher's concern.
At present, industry is made LiMn2O4 and is mainly used electrolytic manganese dioxide as raw material, through mixing with lithium carbonate or lithium hydroxide; Make 800 ℃ of left and right sides high-temperature calcinations then; The quality of the LiMn2O4 product that obtains like this awaits further raising, and major defect is that the electrolytic manganese dioxide powder is made by mechanical disintegration, and its granule-morphology is difficult to control; Be generally amorphous pellets, specific area is bigger.In addition, the impurity content of electrolytic manganese dioxide own is higher, and in crushing process, introduces iron tramp easily because of the plant equipment problem, and these factors are all having a strong impact on the quality of LiMn2O4 product.Therefore; Producing high-quality LiMn2O4 preferably uses spherical mangano-manganic oxide to be raw material; Equally through making with the lithium metal source is baking mixed, guaranteed that on the one hand its spherical structure, specific area are less, help the processing in the battery production process and reduce the capacity attenuation that the manganese dissolving is caused; The synthetic mangano-manganic oxide of wet method can effectively be controlled impurity content on the other hand, helps guaranteeing the cycle performance of battery.
Summary of the invention
In order to solve the technical problem that exists in the prior art, the object of the present invention is to provide a kind of coprecipitation reaction to prepare Mn 3O 4And through joining the spherical structure lithium cell anode material lithium manganate (LiMn that lithium source sintering is processed 2O 4) preparation technology.
The technical scheme that the present invention adopts is following:
The preparation technology of spherical structure lithium cell anode material lithium manganate is characterized in that, step is following:
1., the preparation of raw material
Prepare manganese salt solution, manganese salt is dissolved in processes solution in the hot water, its concentration is 1～3mol/L;
The preparation mass fraction is 20～30% NaOH solution, 10～20% ammonia spirit;
2., spherical Mn 3O 4The preparation of presoma
With the pure water is end liquid, and temperature rises to 50～80 ℃, opens and stirs, and the control speed of agitator adds ammoniacal liquor and NaOH at 60～180r/min, regulates the basicity and the pH of end liquid, makes basicity maintain 5～30g/L, pH 9～12;
With constant flow pump manganese salt solution, ammonia spirit and NaOH solution are added in the agitated reactor of high-speed stirred, the feeding flow is 10～20m in the reactant liquor simultaneously 3The air of/h, the pH of conditioned reaction solution maintains 9～13, and synthesis temperature is 50～80 ℃, and basicity maintains 20～40g/L, and digestion time is 15～30h;
After reacting completely, through washing, filtration, dry spherical Mn 3O 4Presoma;
3., sintering
With spherical Mn 3O 4Presoma, Li source compound be Li in molar ratio: Mn=1: 2 proportioning ball mill mixing is abundant; Speed intensification with 1～10 ℃/min in air is heated; At 500～800 ℃ of calcining at constant temperature 10～30h, cool to room temperature with the furnace, make spherical structure anode material for lithium-ion batteries LiMn 2O 4
Preferably, described manganese salt is a kind of in manganese nitrate, manganese chloride, manganese acetate, the manganese sulfate.
Preferably, described Li source compound is selected from a kind of in lithium hydroxide, lithium acetate, lithium carbonate, the lithium nitrate.
The preparation technology of spherical structure lithium cell anode material lithium manganate of the present invention has proposed with homemade spherical Mn 3O 4For presoma prepares anode material for lithium-ion batteries LiMn 2O 4Preparation technology, synthetic method is simple, process is easy to control, efficient is high, and is with low cost, energy savings and resource are fit to industrialization production.
Description of drawings
For the ease of it will be appreciated by those skilled in the art that the present invention is further described below in conjunction with accompanying drawing.
Fig. 1 is spherical Mn 3O 4The SEM figure of presoma.
Fig. 2 is spherical structure anode material for lithium-ion batteries LiMn 2O 4SEM figure.
Embodiment
Embodiment 1
(1), with manganese sulfate (MnSO 4H 2O) be dissolved in and be made into the solution that manganese content is 60g/L in the deionized water, using deionized water to be made into mass fraction equally is that 23% NaOH (NaOH) solution and mass fraction are 18% ammoniacal liquor (NH4OH) solution.
(2), be end liquid with the pure water, temperature rises to 50 ℃.Open and stir, the control speed of agitator adds ammoniacal liquor and NaOH at 180r/min, regulates the basicity and the pH of end liquid, and control basicity is 25g/L, and pH is 12.
(3), manganese salt solution, ammonia spirit and sodium hydroxide solution are added in the agitated reactor of high-speed stirred, with constant flow pump simultaneously in the reactant liquor feeding flow be 10m 3The air of/h, the pH of conditioned reaction solution maintains 12, and synthesis temperature is 55 ± 1 ℃, and basicity maintains 25g/L, and digestion time is 15h, reaction finishes after wash, filter and be drying to obtain spherical Mn 3O 4Presoma.See also Fig. 1, spherical Mn 3O 4The mobility of particle of presoma is better.
(4), with Mn 3O 4Presoma and Li 2CO 3The Li/Mn=1/2 ball mill mixing is abundant in molar ratio, in air, with the speed intensification heating of 2 ℃/min, at 750 ℃ of calcining at constant temperature 10h, cools to room temperature with the furnace, makes anode material for lithium-ion batteries LiMn 2O 4See also Fig. 2, anode material for lithium-ion batteries LiMn 2O 4Tap density higher.
Embodiment 2
(1), with manganese chloride (MnCl 24H 2O) be dissolved in and be made into the solution that manganese content is 75g/L in the deionized water, using deionized water to be made into mass fraction equally is that 23% NaOH (NaOH) solution and mass fraction are 18% ammoniacal liquor (NH4OH) solution.
(2), be end liquid with the pure water, temperature rises to 60 ℃.Open and stir, the control speed of agitator adds ammoniacal liquor and NaOH at 160r/min, regulates the basicity and the pH of end liquid, and control basicity is 25g/L, and pH is 10.
(3), with constant flow pump with in the parallel agitated reactor that adds high-speed stirred of manganese salt solution, ammonia spirit and sodium hydroxide solution, the feeding flow is 15m in the reactant liquor simultaneously 3The air of/h, the pH of conditioned reaction solution maintains 10; Synthesis temperature is 60 ± 1 ℃; Basicity maintains 25g/L; Digestion time is 15h, and reaction finishes after wash, filter and be drying to obtain spherical Mn 3O 4Presoma.
(4), with Mn 3O 4Presoma and LiNO 3The Li/Mn=1/2 ball mill mixing is abundant in molar ratio, in air, with the speed intensification heating of 4 ℃/min, at 800 ℃ of calcining at constant temperature 14h, cools to room temperature with the furnace, makes anode material for lithium-ion batteries LiMn 2O 4
Embodiment 3
(1), with manganese nitrate (Mn (NO 3) 24H 2O) be dissolved in and be made into the solution that manganese content is 75g/L in the deionized water, using deionized water to be made into mass fraction equally is that 23% NaOH (NaOH) solution and mass fraction are 18% ammoniacal liquor (NH4OH) solution.
(2), be end liquid with the pure water, temperature rises to 70 ℃.Open and stir, the control speed of agitator adds ammoniacal liquor and NaOH at 140r/min, regulates the basicity and the pH of end liquid, and control basicity is 25g/L, and pH is 10.
(3), with constant flow pump with in the parallel agitated reactor that adds high-speed stirred of manganese salt solution, ammonia spirit and sodium hydroxide solution, the feeding flow is 15m in the reactant liquor simultaneously 3The air of/h, the pH of conditioned reaction solution maintains 10; Synthesis temperature is 65 ± 1 ℃; Basicity maintains 25g/L; Digestion time is 15h, and reaction finishes after wash, filter and be drying to obtain spherical Mn 3O 4Presoma.
(4), with Mn 3O 4Presoma and LiOHH 2The Li/Mn=1/2 ball mill mixing is abundant in molar ratio for O, in air, with the speed intensification heating of 6 ℃/min, at 600 ℃ of calcining at constant temperature 22h, cools to room temperature with the furnace, makes anode material for lithium-ion batteries LiMn 2O 4
Embodiment 4
(1), with manganese acetate (Mn (COOH) 24H 2O) be dissolved in and be made into the solution that manganese content is 100g/L in the deionized water, using deionized water to be made into mass fraction equally is that 23% NaOH (NaOH) solution and mass fraction are 18% ammoniacal liquor (NH4OH) solution.
(2), be end liquid with the pure water, temperature rises to 80 ℃.Open and stir, the control speed of agitator adds ammoniacal liquor and NaOH at 120r/min, regulates the basicity and the pH of end liquid, and control basicity is 20g/L, and pH is 11.5.
(3), with constant flow pump with in the parallel agitated reactor that adds high-speed stirred of manganese salt solution, ammonia spirit and sodium hydroxide solution, the feeding flow is 20m in the reactant liquor simultaneously 3The air of/h, the pH of conditioned reaction solution maintains 11.5; Synthesis temperature is 75 ± 1 ℃; Basicity maintains 20g/L; Digestion time is 15h, and reaction finishes after wash, filter and be drying to obtain spherical Mn 3O 4Presoma.
(4), with Mn 3O 4Presoma and LiOHH 2The Li/Mn=1/2 ball mill mixing is abundant in molar ratio for O, in air, with the speed intensification heating of 8 ℃/min, at 600 ℃ of calcining at constant temperature 28h, cools to room temperature with the furnace, makes anode material for lithium-ion batteries LiMn 2O 4
Embodiment 5
(1), with manganese acetate (Mn (CH 3COO) 24H 2O) be dissolved in and be made into the solution that manganese content is 100g/L in the deionized water, using deionized water to be made into mass fraction equally is that 23% NaOH (NaOH) solution and mass fraction are 18% ammoniacal liquor (NH4OH) solution.
(2), be end liquid with the pure water, temperature rises to 50 ℃.Open and stir, the control speed of agitator adds ammoniacal liquor and NaOH at 60r/min, regulates the basicity and the pH of end liquid, and control basicity is 20g/L, and pH is 11.5.
(3), with constant flow pump with in the parallel agitated reactor that adds high-speed stirred of manganese salt solution, ammonia spirit and sodium hydroxide solution, the feeding flow is 20m in the reactant liquor simultaneously 3The air of/h, the pH of conditioned reaction solution maintains 11.5; Synthesis temperature is 55 ± 1 ℃; Basicity maintains 20g/L; Digestion time is 15h, and reaction finishes after wash, filter and be drying to obtain spherical Mn 3O 4Presoma.
(4), with Mn 3O 4Presoma and CH 3COOLi2H 2The Li/Mn=1/2 ball mill mixing is abundant in molar ratio for O, in air, with the speed intensification heating of 10 ℃/min, at 500 ℃ of calcining at constant temperature 30h, cools to room temperature with the furnace, makes anode material for lithium-ion batteries LiMn 2O 4
Above content only is to be given an example and explanation to what the present invention's design did; Under the technical staff in present technique field described specific embodiment is made various modifications or replenish or adopt similar mode to substitute; Only otherwise depart from the design of invention or surmount the defined scope of these claims, all should belong to protection scope of the present invention.

Claims (3)

1. the preparation technology of spherical structure lithium cell anode material lithium manganate is characterized in that, step is following:
1., the preparation of raw material
Prepare manganese salt solution, manganese salt is dissolved in processes solution in the hot water, its concentration is 1～3mol/L;
The preparation mass fraction is 20～30% NaOH solution, 10～20% ammonia spirit;
2., spherical Mn 3O 4The preparation of presoma
With the pure water is end liquid, and temperature rises to 50～80 ℃, opens and stirs, and the control speed of agitator adds ammoniacal liquor and NaOH at 60～180r/min, regulates the basicity and the pH of end liquid, makes basicity maintain 5～30g/L, pH 9～12;
With constant flow pump manganese salt solution, ammonia spirit and NaOH solution are added in the agitated reactor of high-speed stirred, the feeding flow is 10～20m in the reactant liquor simultaneously 3The air of/h, the pH of conditioned reaction solution maintains 9～13, and synthesis temperature is 50～80 ℃, and basicity maintains 20～40g/L, and digestion time is 15～30h;
After reacting completely, through washing, filtration, dry spherical Mn 3O 4Presoma;
3., sintering
With spherical Mn 3O 4Presoma, Li source compound be Li in molar ratio: Mn=1: 2 proportioning ball mill mixing is abundant; Speed intensification with 1～10 ℃/min in air is heated; At 500～800 ℃ of calcining at constant temperature 10～30h, cool to room temperature with the furnace, make spherical structure anode material for lithium-ion batteries LiMn 2O 4
2. the preparation technology of spherical structure lithium cell anode material lithium manganate according to claim 1 is characterized in that, described manganese salt is a kind of in manganese nitrate, manganese chloride, manganese acetate, the manganese sulfate.
3. the preparation technology of spherical structure lithium cell anode material lithium manganate according to claim 1 is characterized in that, described Li source compound is selected from a kind of in lithium hydroxide, lithium acetate, lithium carbonate, the lithium nitrate.
CN2012103054894A 2012-08-24 2012-08-24 Preparation process of anode material lithium manganate of spherical structure for lithium ion battery Pending CN102820462A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106848291A (en) * 2017-03-13 2017-06-13 符策煌 Mangano-manganic oxide is that negative pole LiMn2O4 is the full battery preparation method of positive pole
CN106876672A (en) * 2017-03-06 2017-06-20 符策煌 High-property lithium manganate electrode material and preparation method thereof
CN111217395A (en) * 2020-03-16 2020-06-02 陕西海恩新材料有限责任公司 High-energy-density lithium manganate cathode material and preparation method thereof
CN111342024A (en) * 2020-03-16 2020-06-26 陕西海恩新材料有限责任公司 Long-cycle lithium manganate positive electrode material and preparation method thereof
CN113421998A (en) * 2021-06-21 2021-09-21 宁德新能源科技有限公司 Electrochemical device and electronic device
CN114259961A (en) * 2021-12-24 2022-04-01 贵州大龙汇成新材料有限公司 System and method for improving capacity of lithium battery anode material precursor and regulating and controlling particle size distribution of precursor
CN115180651A (en) * 2022-09-09 2022-10-14 河南科隆新能源股份有限公司 Preparation method of manganous-manganic oxide material with controllable particle size for lithium manganate

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CN101764211A (en) * 2009-10-14 2010-06-30 孙琦 Preparation method of spherical lithium manganese for lithium-ion battery cathode material
CN102336441A (en) * 2011-06-29 2012-02-01 金瑞新材料科技股份有限公司 Method for preparing lithium manganate used as lithium ion battery anode material by using trimanganese tetroxide
CN102491422A (en) * 2011-12-26 2012-06-13 湖南汇通科技有限责任公司 Spherical manganic manganous oxide and its preparation method
CN102502850A (en) * 2011-11-04 2012-06-20 安徽亚兰德新能源材料股份有限公司 Preparation method of lithium manganate precursor spherical manganese hydroxide

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JPH06215771A (en) * 1993-01-19 1994-08-05 Dowa Mining Co Ltd Preparation of positive pole active material for lithium secondary battery
CN1447464A (en) * 2003-04-26 2003-10-08 清华大学 Method for preparing spherical lighium manganate anode material of lighium ion batteries
CN1562771A (en) * 2004-04-07 2005-01-12 中信国安盟固利电源技术有限公司 Spherical shaped lithium manganate and preparation method
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106876672A (en) * 2017-03-06 2017-06-20 符策煌 High-property lithium manganate electrode material and preparation method thereof
CN106848291A (en) * 2017-03-13 2017-06-13 符策煌 Mangano-manganic oxide is that negative pole LiMn2O4 is the full battery preparation method of positive pole
CN111217395A (en) * 2020-03-16 2020-06-02 陕西海恩新材料有限责任公司 High-energy-density lithium manganate cathode material and preparation method thereof
CN111342024A (en) * 2020-03-16 2020-06-26 陕西海恩新材料有限责任公司 Long-cycle lithium manganate positive electrode material and preparation method thereof
CN113421998A (en) * 2021-06-21 2021-09-21 宁德新能源科技有限公司 Electrochemical device and electronic device
CN113421998B (en) * 2021-06-21 2022-07-08 宁德新能源科技有限公司 Electrochemical device and electronic device
CN114259961A (en) * 2021-12-24 2022-04-01 贵州大龙汇成新材料有限公司 System and method for improving capacity of lithium battery anode material precursor and regulating and controlling particle size distribution of precursor
CN115180651A (en) * 2022-09-09 2022-10-14 河南科隆新能源股份有限公司 Preparation method of manganous-manganic oxide material with controllable particle size for lithium manganate

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