CN105271423A - Method for synthesizing highly-pure nanometer lithium manganate at low temperature - Google Patents
Method for synthesizing highly-pure nanometer lithium manganate at low temperature Download PDFInfo
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- CN105271423A CN105271423A CN201510658575.7A CN201510658575A CN105271423A CN 105271423 A CN105271423 A CN 105271423A CN 201510658575 A CN201510658575 A CN 201510658575A CN 105271423 A CN105271423 A CN 105271423A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
A method for synthesizing highly-pure nanometer lithium manganate at low temperature comprises employing potassium permanganate, manganese sulfate and lithium hydroxide as raw materials, mixing according to a ratio, performing hydrothermal reaction to directly prepare the highly-pure lithium manganate through one step. Lithium manganate prepared according to the method is nanometer level particle, and the particle size distribution is uniform. Compared with a conventional method for preparing lithium manganate through a high-temperature solid-phase reaction, the method possesses the characteristics of being simple in technology step, low in reaction temperature, short in reaction time, low in equipment requirement, less in energy consumption and strong in repeatability.
Description
Technical field
The present invention relates to technical field of lithium ion battery positive pole material preparation, particularly a kind of processing method of low temperature synthesis high-purity nm lithium manganate.
Background technology
In order to meet the demand in more high storage capacity, the high rate performance of lithium ion battery and the energy density of lithium ion must improve, and this impels researchist to work out the negative or positive electrode material of renewal.And as the lithium manganate of one of several anode material for lithium-ion batteries instantly most with prospects, the advantages such as, environmentally safe, cold cycle performance cheap by means of it are good, obtain the extensive attention of investigators.But tradition prepares the high temperature solid-state method of lithium manganate material, its long reaction time, temperature of reaction are high, particle size distributing inhomogeneity and particle size is generally micron order.And nano material has special nanometer size effect, if the size of lithium manganate particle is controlled in nano level, lithium ion and the electronics the evolving path in lithium manganate will greatly shorten, and show excellent high rate performance.Secondly, because nano material has special surface effects, the lithium manganate of nano-scale is easier to surface modification.
Through finding the retrieval of prior art, Patent document number CN102790210A discloses a kind of method preparing submicron order lithium manganate.This technology prepare the hydrothermal temperature of lithium manganate up to 380 DEG C ~ 420 DEG C, in reactor, pressure needs to be adjusted to 22MPa ~ 40MPa, and the reactor that market can meet this reaction conditions is expensive, and hydro-thermal reaction danger coefficient under this condition is higher.
Patent document number CN10478672A discloses a kind of method of manganese oxide and spinel lithium manganate lithium ion battery and preparation thereof, this technology adopts two step hydro-thermal and high temperature solid-state methods, by adding reductive agent in hydrothermal system, realize the transformation of manganese oxide nano-chip arrays to nano-wire array with tensio-active agent; Add lithium source in being reacted by high temperature solid-state method, realize the preparation of manganese oxide and lithium manganate having spinel structure nano wire, but the method that this technology prepares lithium manganate is still high temperature solid-state method, hydro-thermal reaction is only for the preparation of the precursor of high temperature solid state reaction.
Patent document number CN104752686A discloses a kind of method adopting conventional high-temperature solid phase method to prepare lithium manganate, and this technology is prepared lithium manganate and adopted raw material MnCO
3, Li
2cO
3mixing and ball milling by a certain percentage, after sieving, is slowly warming up to 600 DEG C, insulation 6h, then is warming up to 800 DEG C ~ 850 DEG C, insulation 18h; This technical matters process is complicated, does not overcome that conventional solid-state method long reaction time, energy consumption are many, the inhomogenous shortcoming of particle size.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, a kind of low temperature is the object of the present invention is to provide to synthesize the processing method of high-purity nm lithium manganate, prepared lithium manganate is nano-scale particle, purity is high, excellent performance and particle size distribution is homogeneous, has that processing step is simple, temperature of reaction is low, the reaction times is short, low for equipment requirements, energy consumption is few, repeatable strong feature.
In order to achieve the above object, the technical scheme that the present invention takes is:
A processing method for low temperature synthesis high-purity nm lithium manganate, its step is as follows:
Step one: by potassium permanganate, manganous sulfate, lithium hydroxide according to mol ratio (0.7-1.1): (1.9-2.3): (22-34) is dissolved in deionized water, mixes, and is configured to reaction solution;
Step 2: reaction solution step one configured is placed in water heating kettle and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 90-120 DEG C, and the reaction times is 3-12h, to be cooled after room temperature, through cleaning, suction filtration, drying, separation, obtains lithium manganate.
Compared with prior art, beneficial effect of the present invention is:
The present invention with potassium permanganate, manganous sulfate, lithium hydroxide for raw material, high purity lithium manganate has directly been prepared by hydro-thermal reaction one step, and obtained lithium manganate particle is nano-scale particle, particle size distribution is homogeneous, be applicable to the positive electrode material preparing lithium ion battery, adopt high temperature solid state reaction to prepare compared with the method for lithium manganate with tradition, the inventive method has that processing step is simple, temperature of reaction is low, the reaction times is short, low for equipment requirements, energy consumption is few, repeatable strong feature.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of high-purity lithium manganate electrode prepared by the present invention.
Fig. 2 is scanning electron microscope (SEM) the microscopic appearance figure of high-purity lithium manganate electrode prepared by the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment one
Step one: 0.9mmol potassium permanganate, 2.1mmol manganous sulfate, 34mmol lithium hydroxide are dissolved in deionized water, mix, be configured to the reaction solution of 80mL;
Step 2: reaction solution step one configured is placed in 100mL water heating kettle and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 90 DEG C, and the reaction times is 6h, to be cooled after room temperature, through cleaning, suction filtration, drying, separation, obtains lithium manganate.
See Fig. 1, the purity of nanometer lithium manganate prepared by the present embodiment is about 99.6%.
See Fig. 2, lithium manganate prepared by the present embodiment is nano level, and size is about 50 nanometers, and its distribution of sizes is homogeneous.
Embodiment two
Step one: 1.1mmol potassium permanganate, 1.9mmol manganous sulfate, 30mmol lithium hydroxide are dissolved in deionized water, mix, be configured to the reaction solution of 80mL;
Step 2: reaction solution step one configured is placed in 100mL water heating kettle and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 100 DEG C, and the reaction times is 9h, to be cooled after room temperature, through cleaning, suction filtration, drying, separation, obtains lithium manganate.
Embodiment three
Step one: 1.0mmol potassium permanganate, 2.0mmol manganous sulfate, 26mmol lithium hydroxide are dissolved in deionized water, mix, be configured to the reaction solution of 80mL;
Step 2: reaction solution step one configured is placed in 100mL water heating kettle and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 110 DEG C, and the reaction times is 3h, to be cooled after room temperature, through cleaning, suction filtration, drying, separation, obtains lithium manganate.
Embodiment four
Step one: 0.7mmol potassium permanganate, 2.3mmol manganous sulfate, 22mmol lithium hydroxide are dissolved in deionized water, mix, be configured to the reaction solution of 80mL;
Step 2: reaction solution step one configured is placed in 100mL water heating kettle and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 120 DEG C, and the reaction times is 12h, to be cooled after room temperature, through cleaning, suction filtration, drying, separation, obtains lithium manganate.
Claims (5)
1. a processing method for low temperature synthesis high-purity nm lithium manganate, it is characterized in that, step is as follows:
Step one: by potassium permanganate, manganous sulfate, lithium hydroxide according to mol ratio (0.7-1.1): (1.9-2.3): (22-34) is dissolved in deionized water, mixes, and is configured to reaction solution;
Step 2: reaction solution step one configured is placed in water heating kettle and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 90-120 DEG C, and the reaction times is 3-12h, to be cooled after room temperature, through cleaning, suction filtration, drying, separation, obtains lithium manganate.
2. the processing method of a kind of low temperature synthesis high-purity nm lithium manganate according to claim 1, it is characterized in that, step is as follows:
Step one: 0.9mmol potassium permanganate, 2.1mmol manganous sulfate, 34mmol lithium hydroxide are dissolved in deionized water, mix, be configured to the reaction solution of 80mL;
Step 2: reaction solution step one configured is placed in 100mL water heating kettle and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 90 DEG C, and the reaction times is 6h, to be cooled after room temperature, through cleaning, suction filtration, drying, separation, obtains lithium manganate.
3. the processing method of a kind of low temperature synthesis high-purity nm lithium manganate according to claim 1, it is characterized in that, step is as follows:
Step one: 1.1mmol potassium permanganate, 1.9mmol manganous sulfate, 30mmol lithium hydroxide are dissolved in deionized water, mix, be configured to the reaction solution of 80mL;
Step 2: reaction solution step one configured is placed in 100mL water heating kettle and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 100 DEG C, and the reaction times is 9h, to be cooled after room temperature, through cleaning, suction filtration, drying, separation, obtains lithium manganate.
4. the processing method of a kind of low temperature synthesis high-purity nm lithium manganate according to claim 1, it is characterized in that, step is as follows:
Step one: 1.0mmol potassium permanganate, 2.0mmol manganous sulfate, 26mmol lithium hydroxide are dissolved in deionized water, mix, be configured to the reaction solution of 80mL;
Step 2: reaction solution step one configured is placed in 100mL water heating kettle and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 110 DEG C, and the reaction times is 3h, to be cooled after room temperature, through cleaning, suction filtration, drying, separation, obtains lithium manganate.
5. the processing method of a kind of low temperature synthesis high-purity nm lithium manganate according to claim 1, it is characterized in that, step is as follows:
Step one: 0.7mmol potassium permanganate, 2.3mmol manganous sulfate, 22mmol lithium hydroxide are dissolved in deionized water, mix, be configured to the reaction solution of 80mL;
Step 2: reaction solution step one configured is placed in 100mL water heating kettle and carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 120 DEG C, and the reaction times is 12h, to be cooled after room temperature, through cleaning, suction filtration, drying, separation, obtains lithium manganate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108134076A (en) * | 2017-12-18 | 2018-06-08 | 常州大学 | A kind of preparation method and application of spinel lithium manganate |
| CN108529682A (en) * | 2018-05-07 | 2018-09-14 | 陕西科技大学 | A kind of sheet LiMn2O4 and preparation method thereof |
| CN115818581A (en) * | 2022-12-19 | 2023-03-21 | 无锡中天固废处置有限公司 | Comprehensive utilization method of manganese-containing waste sulfuric acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108134076A (en) * | 2017-12-18 | 2018-06-08 | 常州大学 | A kind of preparation method and application of spinel lithium manganate |
| CN108529682A (en) * | 2018-05-07 | 2018-09-14 | 陕西科技大学 | A kind of sheet LiMn2O4 and preparation method thereof |
| CN115818581A (en) * | 2022-12-19 | 2023-03-21 | 无锡中天固废处置有限公司 | Comprehensive utilization method of manganese-containing waste sulfuric acid |
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Application publication date: 20160127 |