CN112978789A - Method for producing lithium titanate by high-temperature melting method - Google Patents
Method for producing lithium titanate by high-temperature melting method Download PDFInfo
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- CN112978789A CN112978789A CN202110167887.3A CN202110167887A CN112978789A CN 112978789 A CN112978789 A CN 112978789A CN 202110167887 A CN202110167887 A CN 202110167887A CN 112978789 A CN112978789 A CN 112978789A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/04—Crucible or pot furnaces adapted for treating the charge in vacuum or special atmosphere
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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 discloses a method for producing lithium titanate by a high-temperature melting method, which comprises the following steps: uniformly mixing lithium hydroxide and anatase titanium dioxide in a molar ratio of 4:5 or lithium carbonate and anatase titanium dioxide in a molar ratio of 2: 5; pouring the materials into a high-temperature reaction container, vacuumizing a reaction cavity of the high-temperature reaction container to 5-10 Pa, starting heating, and maintaining the materials in the high-temperature reaction container for 1-2 hours at 1650-1750 ℃ for liquid phase reaction; pumping out reaction gas generated in the heating process by using a vacuum pump, and maintaining the air pressure in the reaction cavity at 5-10 Pa; after the reaction is finished, pouring the lithium titanate melt generated by the reaction into a cooling mold through a furnace, standing and cooling, taking out the lithium titanate solid, crushing, and packaging; the method has the advantages of short liquid phase reaction time, few process links, low relative cost, thorough product synthesis reaction and higher purity of the generated lithium titanate.
Description
Technical Field
The invention relates to a method for producing lithium titanate, in particular to a method for producing lithium titanate by a high-temperature melting method.
Background
The lithium titanate negative electrode battery has the cycle life as long as 2 ten thousand times and is used as an energy storage battery, and the energy storage cost of the lithium titanate battery is 5000 yuan/DEG of electricity at present. With the further reduction of the cost, the energy storage cost can be reduced by 3000 yuan/degree electricity. Calculated according to the cycle life of 20000 times, the material can work for 60 years (charge and discharge once a day), and the average depreciation cost is 0.15 yuan/degree. In addition, the cost of the existing photovoltaic power generation is 0.1 yuan/degree, and the cost of the photovoltaic power generation for supplying power all day is lower than 0.3 yuan/degree. And the power generation cost of the current coal-fired thermal power generating set is about 0.4 yuan/degree. Therefore, the lithium titanate battery has advantages as an energy storage battery, and with the exhaustion of world energy sources, the lithium titanate battery can be used as an energy storage battery with a long cycle life.
At present, the specific energy of a lithium titanate battery is 50-90 wh/kg, 10000 kilowatt-hour electric energy is stored by 160 tons of batteries on average, and if one photovoltaic or wind power energy storage is 1000 kilowatt-hour electric energy (namely 40 kilowatt-hours of supplied energy), 16 kiloton lithium titanate batteries are needed. 0.25-0.3 tons of lithium titanate negative electrode materials are needed for each ton of lithium titanate battery, and 4-5 tons of lithium titanate materials are needed for storing 1000 ten thousand kilowatt-hours of electric energy. One of the methods for reducing the lithium titanate battery is to reduce the production cost of the lithium carbonate material.
Lithium titanate (Li)4Ti5O12) Synthesized by raw materials of titanium dioxide and lithium hydroxide. The current production method is to adopt a solid phase method for preparation, and lithium carbonate and anatase are impacted, ball-milled and mixed for a long time (8-12 hours), and sintered for 8 hours at 800 ℃ in air to form a white powder product. And (4) performing solid-phase reaction by using a high-temperature energy ball mill. Besides, the lithium titanate material can be prepared by sol-gel method, hydrothermal method, spray pyrolysis method, molten salt method and the like. The current main problems are complex process and high cost. And the lithium titanate material synthesized by the solid-phase method has low uniformity, slow solid-phase reaction, serious product agglomeration phenomenon and poor electrochemical performance.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for producing lithium titanate by a high-temperature melting method, which has the advantages of short liquid phase reaction time, few process links, low relative cost, thorough product synthesis reaction and high purity of the generated lithium titanate.
In order to solve the technical problems, the technical scheme of the invention is as follows: a method for producing lithium titanate by a high-temperature melting method comprises the following steps:
step one, taking lithium hydroxide and anatase type titanium dioxide with a molar ratio of 4:5 as raw materials, and uniformly mixing;
or taking lithium carbonate and anatase titanium dioxide with the molar ratio of 2:5 as raw materials, and uniformly mixing;
step two, pouring the uniformly mixed materials in the step one into a high-temperature reaction container, vacuumizing a reaction cavity of the high-temperature reaction container to 5-10 Pa, starting heating, and maintaining the materials in the high-temperature reaction container for 1-2 hours at 1650-1750 ℃ for liquid phase reaction;
pumping out reaction gas generated in the heating process by using a vacuum pump communicated with a reaction cavity of the high-temperature reaction container, and maintaining the air pressure in the reaction cavity at 5-10 Pa;
and step four, after the reaction is finished, pouring the lithium titanate melt generated by the reaction into a cooling mold through a furnace, standing and cooling, taking out the lithium titanate solid, crushing, and packaging.
As a preferred technical scheme, the high-temperature reaction container comprises a medium-frequency induction heating high-temperature furnace, the high-temperature furnace comprises a furnace body and a furnace cover, a graphite crucible liner is arranged in the furnace body, a medium-frequency induction coil is sleeved outside the graphite crucible liner, a furnace cover sealing cavity is formed between the inner wall of the graphite crucible liner and the furnace cover, a crucible external sealing cavity is formed between the outer wall of the graphite crucible liner and the furnace body, a furnace cover vacuum connecting pipe and a vacuum breaking valve are arranged on the furnace cover, and a furnace body vacuum connecting pipe and an inert gas valve are arranged on the furnace body.
As a preferred technical scheme, the reaction chamber of the high-temperature reaction container comprises an inner chamber of the graphite crucible inner container, the furnace cover sealing chamber comprises the reaction chamber of the high-temperature reaction container and an inner chamber of the furnace cover, and in the second step, the furnace cover sealing chamber is vacuumized to 5-10 Pa air pressure.
As a preferred technical scheme, in the second step, the materials are poured into a graphite crucible inner container of a high-temperature reaction container, the furnace cover of the high-temperature furnace is closed, a vacuum pump is used for vacuumizing an external sealed cavity of the crucible to 10-100 Pa of air pressure, then an inert gas valve is used for filling argon into the external sealed cavity of the crucible to 0.08-0.1 MPa of air pressure, and then medium-frequency induction heating is started.
As a preferable technical scheme, in the fourth step, after the reaction is completed, the vacuum pump connected with the furnace cover vacuum connecting pipe stops working, argon is filled into the furnace cover sealing cavity through the vacuum breaking valve on the furnace cover until the pressure is 0.09-0.11 MPa, and then the furnace cover is opened.
As a preferable technical scheme, lithium hydroxide and anatase type titanium dioxide with a molar ratio of 4:5 are taken as raw materials, and the chemical formula of liquid phase reaction is 4LiOH +5TiO2＝Li4Ti5O12+2H2O。
As a preferable technical scheme, lithium carbonate and anatase titanium dioxide with the molar ratio of 2:5 are taken as raw materials, and the chemical formula of liquid phase reaction is 2Li2CO3+5TiO2＝Li4Ti5O12+2CO2。
As a preferable technical solution, in the fourth step, the cooling mold is a graphite cooling mold.
As a preferable technical scheme, in the first step, the materials are mixed by using a common stirrer or a ball mill.
Due to the adoption of the technical scheme, the method for producing the lithium titanate by the high-temperature melting method comprises the following steps: step one, taking lithium hydroxide and anatase type titanium dioxide with a molar ratio of 4:5 as raw materials, and uniformly mixing; or taking lithium carbonate and anatase titanium dioxide with the molar ratio of 2:5 as raw materials, and uniformly mixing; step two, pouring the uniformly mixed materials in the step one into a high-temperature reaction container, vacuumizing a reaction cavity of the high-temperature reaction container to 5-10 Pa, starting heating, and maintaining the materials in the high-temperature reaction container for 1-2 hours at 1650-1750 ℃ for liquid phase reaction; pumping out reaction gas generated in the heating process by using a vacuum pump communicated with a reaction cavity of the high-temperature reaction container, and maintaining the air pressure in the reaction cavity at 5-10 Pa; step four, after the reaction is finished, pouring the lithium titanate melt generated by the reaction into a cooling mold through a converter, standing and cooling, taking out the lithium titanate solid, crushing, and packaging; the method has the advantages of short liquid phase reaction time, few process links, low relative cost, thorough product synthesis reaction and higher purity of the generated lithium titanate.
Drawings
The drawings are only for purposes of illustrating and explaining the present invention and are not to be construed as limiting the scope of the present invention. Wherein:
FIG. 1 is a schematic structural view of a high temperature furnace according to an embodiment of the present invention;
FIG. 2 is a sectional view of a high temperature furnace according to an embodiment of the present invention;
FIG. 3 is a schematic layout of a high temperature reaction vessel and associated fittings according to an embodiment of the present invention;
in the figure: 11-a furnace body; 12-furnace cover; 13-graphite crucible inner container; 14-medium frequency induction coil; 15-furnace lid vacuum connection tube; 16-breaking the vacuum valve; 17-furnace body vacuum connecting pipe; 18-inert gas valve; 21-a working platform; 22-track; 23-a walking vehicle; 24-a chain; 25-a diversion trench; 31-a furnace cover sealing cavity; 32-the crucible exterior seals the cavity.
Detailed Description
The invention is further illustrated below with reference to the figures and examples. In the following detailed description, certain exemplary embodiments of the present invention are described by way of illustration only. Needless to say, a person skilled in the art realizes that the described embodiments can be modified in various different ways without departing from the spirit and scope of the present invention. Accordingly, the drawings and description are illustrative in nature and not intended to limit the scope of the claims.
A method for producing lithium titanate by a high-temperature melting method comprises the following steps:
step one, taking lithium hydroxide and anatase type titanium dioxide with a molar ratio of 4:5 as raw materials, and uniformly mixing;
or taking lithium carbonate and anatase titanium dioxide with the molar ratio of 2:5 as raw materials, and uniformly mixing; mixing the materials by using a common stirrer or a ball mill;
step two, pouring the uniformly mixed materials in the step one into a high-temperature reaction container, vacuumizing a reaction cavity of the high-temperature reaction container to 5-10 Pa, starting heating, and maintaining the materials in the high-temperature reaction container for 1-2 hours at 1650-1750 ℃ for liquid phase reaction;
pumping out reaction gas generated in the heating process by using a vacuum pump communicated with a reaction cavity of the high-temperature reaction container, and maintaining the air pressure in the reaction cavity at 5-10 Pa;
and step four, after the reaction is finished, pouring the lithium titanate melt generated by the reaction into a cooling mould through a furnace tilting, wherein the cooling mould is a graphite cooling mould, standing and cooling the lithium titanate melt, taking out the lithium titanate solid, crushing the lithium titanate solid, and packaging the lithium titanate solid.
As shown in fig. 1, fig. 2 and fig. 3, the high-temperature reaction vessel includes a high-temperature furnace of medium-frequency induction heating, the high-temperature furnace includes a furnace body 11 and a furnace cover 12, a graphite crucible liner 13 is arranged in the furnace body 11, a medium-frequency induction coil 14 is sleeved outside the graphite crucible liner 13, a furnace cover 12 sealing cavity is formed between the inner wall of the graphite crucible liner 13 and the furnace cover 12, a crucible external sealing cavity 32 is formed between the outer wall of the graphite crucible liner 13 and the furnace body 11, a furnace cover 12 vacuum connecting pipe and a vacuum breaking valve 16 are arranged on the furnace cover 12, and a furnace body 11 vacuum connecting pipe and an inert gas valve 18 are arranged on the furnace body 11. The high-temperature furnace is arranged on the working platform 21, a rail 22 is arranged on the working platform 21 at one side of the high-temperature furnace, a walking vehicle 23 is arranged on the rail 22, a chain 24 is arranged between the walking vehicle 23 and the furnace cover 12 of the high-temperature furnace, the walking vehicle 23 moves on the rail 22, and the furnace cover 12 is pulled to be opened or closed through the chain 24; a flow guide groove 25 is arranged on the working platform 21 at the other side of the high-temperature furnace, so that the solution in the high-temperature furnace can be poured out conveniently.
And in the second step, the reaction cavity of the high-temperature reaction container comprises the inner cavity of the graphite crucible inner container 13, the sealing cavity of the furnace cover 12 comprises the reaction cavity of the high-temperature reaction container and the inner cavity of the furnace cover 12, and the sealing cavity of the furnace cover 12 is vacuumized to 5-10 Pa air pressure. The sealed cavity of the furnace cover 12 reduces the oxidation of the crucible and the raw materials in a vacuum pumping mode, and simultaneously pumps out water vapor or carbon dioxide generated in the reaction process.
In the second step, the materials are poured into a graphite crucible inner container 13 of a high-temperature reaction container, the furnace cover 12 of the high-temperature furnace is closed, the crucible outer sealing cavity 32 is firstly vacuumized to 10-100 Pa air pressure by using a vacuum pump, then argon is filled into the crucible outer sealing cavity 32 to 0.08-0.1 MPa air pressure through the inert gas valve 18, and then medium-frequency induction heating is started. Argon is filled into the crucible external sealing cavity 32, so as to protect the outer wall of the graphite crucible inner container 13 and prevent oxidation at high temperature; the electromagnetic stirring force of the medium-frequency induction heating high-temperature furnace is utilized to ensure that the melted materials are fully mixed and reacted, and the production period is short.
In the fourth step, after the reaction is finished, the vacuum pump connected with the vacuum connecting pipe of the furnace cover 12 stops working, argon is filled into the sealing cavity of the furnace cover 12 through the vacuum breaking valve 16 on the furnace cover 12 until the air pressure is 0.09-0.11 MPa, and then the furnace cover 12 is opened.
Taking lithium hydroxide and anatase titanium dioxide with a molar ratio of 4:5 as raw materials, and the chemical formula of liquid phase reaction is 4LiOH +5TiO2＝Li4Ti5O12+2H2O。
Taking lithium carbonate and anatase titanium dioxide with the molar ratio of 2:5 as raw materials, and carrying out liquid phase reaction with the chemical formula of 2Li2CO3+5TiO2＝Li4Ti5O12+2CO2。
Whether or not lithium hydroxide is selectedThe lithium carbonate is used as a raw material, and the lithium carbonate is carried out in two steps in the liquid phase reaction process, so that an intermediate product, namely lithium metatitanate Li is generated2TiO3Further synthesizing lithium titanate Li4Ti5O12The chemical formula is as follows:
2Li2TiO3+3TiO2＝Li4Ti5O12
when lithium hydroxide is used as a lithium source, only water vapor is discharged in the synthesis reaction process; when lithium carbonate is used as a lithium source, carbon dioxide is also discharged in the synthesis reaction process.
In the method for producing lithium titanate by the high-temperature melting method, a lithium source of a synthetic raw material is lithium hydroxide or lithium carbonate, and a titanium source is titanium dioxide; the high-temperature reaction vessel is a graphite crucible; the heating method is heating by an inert gas protection type medium frequency induction furnace, and has the structural configuration of sealed vacuum pumping and sealed inert gas filling, and the high temperature furnace also has the functions of uncapping for feeding and uncapping for pouring molten solution.
The method for producing lithium titanate by the high-temperature melting method has the main advantages that:
1) compared with the molten salt synthesis method, the method can realize liquid phase synthesis without adding molten salt with low melting point, and the molten salt synthesis method has complex molten salt separation process, incomplete separation and low product purity.
2) Compared with a solid-phase synthesis method, the solid-phase synthesis method requires 8-12 hours of ball-milling impact mixing, the sintering reaction time of a solid-phase container is long, the reaction is insufficient, and the product performance is poor; compared with the solid phase method, the method has less process links.
3) The method has the advantages of short liquid phase reaction time, few process links, relatively low cost, thorough product synthesis reaction and higher purity of the generated lithium titanate.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A method for producing lithium titanate by a high-temperature melting method is characterized by comprising the following steps:
step one, taking lithium hydroxide and anatase type titanium dioxide with a molar ratio of 4:5 as raw materials, and uniformly mixing;
or taking lithium carbonate and anatase titanium dioxide with the molar ratio of 2:5 as raw materials, and uniformly mixing;
step two, pouring the uniformly mixed materials in the step one into a high-temperature reaction container, vacuumizing a reaction cavity of the high-temperature reaction container to 5-10 Pa, starting heating, and maintaining the materials in the high-temperature reaction container for 1-2 hours at 1650-1750 ℃ for liquid phase reaction;
pumping out reaction gas generated in the heating process by using a vacuum pump communicated with a reaction cavity of the high-temperature reaction container, and maintaining the air pressure in the reaction cavity at 5-10 Pa;
and step four, after the reaction is finished, pouring the lithium titanate melt generated by the reaction into a cooling mold through a furnace, standing and cooling, taking out the lithium titanate solid, crushing, and packaging.
2. The method for producing lithium titanate by using the high-temperature melting method according to claim 1, wherein the high-temperature reaction vessel comprises a medium-frequency induction heating high-temperature furnace, the high-temperature furnace comprises a furnace body and a furnace cover, a graphite crucible inner container is arranged in the furnace body, a medium-frequency induction coil is sleeved outside the graphite crucible inner container, a furnace cover sealing cavity is formed between the inner wall of the graphite crucible inner container and the furnace cover, a crucible outer sealing cavity is formed between the outer wall of the graphite crucible inner container and the furnace body, a furnace cover vacuum connecting pipe and a vacuum breaking valve are arranged on the furnace cover, and a furnace body vacuum connecting pipe and an inert gas valve are arranged on the furnace body.
3. The method for producing lithium titanate by using the high-temperature melting method according to claim 2, wherein the reaction chamber of the high-temperature reaction vessel includes an inner chamber of the graphite crucible inner container, the furnace cover sealing chamber includes the reaction chamber of the high-temperature reaction vessel and an inner chamber of the furnace cover, and in the second step, the furnace cover sealing chamber is evacuated to 5-10 Pa.
4. The method for producing lithium titanate by high-temperature melting according to claim 2, wherein in the second step, the material is poured into a graphite crucible inner container of a high-temperature reaction vessel, the furnace cover of the high-temperature furnace is closed, a vacuum pump is used to evacuate an external sealed cavity of the crucible to 10-100 Pa, then an inert gas valve is used to fill argon gas into the external sealed cavity of the crucible to 0.08-0.1 MPa, and then medium-frequency induction heating is started.
5. The method for producing lithium titanate by high-temperature melting according to claim 2, wherein in the fourth step, after the reaction is completed, the vacuum pump connected to the furnace cover vacuum connection pipe is stopped, argon gas is filled into the furnace cover sealing cavity through the vacuum breaking valve on the furnace cover to reach a pressure of 0.09-0.11 MPa, and then the furnace cover is opened.
6. The method for producing lithium titanate by high-temperature melting according to claim 1, wherein lithium hydroxide and anatase titanium dioxide are used as raw materials in a molar ratio of 4:5, and the chemical formula of the liquid-phase reaction is 4LiOH +5TiO2＝Li4Ti5O12+2H2O。
7. The method of manufacturing lithium titanate by high temperature melting process according to claim 1, wherein the molar ratio of lithium carbonate to anatase dioxygen is 2:5Titanium oxide as a raw material, and the chemical formula of the liquid phase reaction is 2Li2CO3+5TiO2＝Li4Ti5O12+2CO2。
8. The process for producing lithium titanate by the high temperature melting method according to claim 1, wherein in the fourth step, the cooling mold is a graphite cooling mold.
9. The method for producing lithium titanate by a high-temperature melting process according to any one of claims 1 to 8, wherein in the first step, the materials are mixed by a common stirrer or a ball mill.
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Application publication date: 20210618 |
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