CN110980775A - Production method for producing multi-grade lithium carbonate through continuous carbonization - Google Patents
Production method for producing multi-grade lithium carbonate through continuous carbonization Download PDFInfo
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- CN110980775A CN110980775A CN201911220647.4A CN201911220647A CN110980775A CN 110980775 A CN110980775 A CN 110980775A CN 201911220647 A CN201911220647 A CN 201911220647A CN 110980775 A CN110980775 A CN 110980775A
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- lithium carbonate
- carbonization
- carbon dioxide
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- lithium hydroxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a production method for producing multi-grade lithium carbonate by continuous carbonization, which comprises the steps of placing lithium hydroxide mother liquor into a mother liquor tank and dissolving the lithium hydroxide mother liquor; then the lithium hydroxide solution in the mother liquor tank flows into at least a 3-stage carbonization reactor, and carbon dioxide is introduced into the carbonization reactor to react with the lithium hydroxide; and finally, centrifugally separating the reaction product by a centrifugal machine, rinsing and centrifuging, and then, connecting into a drier for heating to obtain a lithium carbonate finished product. The invention realizes the continuous production of lithium carbonate, and the production system has high productivity, high production efficiency, low production cost and stable product quality.
Description
Technical Field
The invention relates to the technical field of lithium carbonate production, in particular to a production method for producing multi-grade lithium carbonate through continuous carbonization.
Background
With the rapid development of low-carbon economy such as mobile communication equipment and green new energy industry, the novel lithium power automobile industry rises rapidly, and the demand for lithium batteries is larger and larger. Lithium cobaltate, lithium manganate and lithium nickelate are the first choice of the positive electrode material of the lithium ion storage battery due to the advantages of good thermal stability, cyclicity, safety, environmental protection and the like. Lithium carbonate is used as a key raw material for producing lithium cobaltate, lithium manganate and lithium nickelate, and the demand is increasing day by day. Meanwhile, the lithium carbonate is applied to semiconductors, ceramics, televisions, medicines, atomic energy industry, chemical analysis and cement flocculants. However, lithium cobaltate, lithium manganate and lithium nickelate are expensive, and the cost reduction of the production cost of lithium carbonate can indirectly reduce the cost of the three battery materials and the cost of other application fields related to lithium carbonate.
The common preparation method of lithium carbonate is salt lake extraction or lithium ore is used for producing lithium carbonate, but in the prior art, the quality grade of the produced lithium carbonate is not high, and the production flow is long. In addition, in the operation process, the lithium carbonate is easy to crystallize and scab on the wall of the reactor, and needs to be treated regularly, so that time and labor are wasted, the utilization rate of equipment is low, and the waste of lithium carbonate products is caused.
Disclosure of Invention
The invention aims to provide a multi-grade lithium carbonate production system, aims to solve the problem that the yield and the purity cannot be guaranteed in the conventional lithium carbonate production process, and has the characteristics of high utilization rate of carbon dioxide and production of multi-grade products by one production line. The technical scheme adopted for achieving the purpose of the invention is as follows:
a production method for producing multi-grade lithium carbonate by continuous carbonization comprises the following steps:
(1) putting the lithium hydroxide mother liquor into a mother liquor tank, and dissolving the lithium hydroxide mother liquor;
(2) enabling the lithium hydroxide solution in the mother liquor tank to flow into at least a 3-stage carbonization reactor, and introducing carbon dioxide into the carbonization reactor to react with lithium hydroxide;
(3) centrifugally separating the reaction product by a centrifugal machine, rinsing and centrifuging, and then connecting into a drier for heating to obtain a lithium carbonate finished product;
the carbon dioxide is converted into carbon dioxide at normal temperature and normal pressure in a low-temperature state by a vaporizer in advance, and then is introduced into a carbonization reactor;
the temperature of the gasified carbon dioxide is 0-30 ℃, the pressure is 0.1-0.5Mpa, and the flow is 0.1-1 t/h;
the lithium hydroxide is represented by Li2The O equivalent weight concentration is 10-50 g/L;
in the carbonization reaction, the reaction temperature is between 50 and 90 ℃, and the pressure is between 0.1 and 0.5 Mpa.
Preferably, the carbon dioxide continuously enters the carbonization reactor, the residual carbon dioxide after the first-stage reaction overflows to the second-stage reactor, the residual carbon dioxide after the second-stage reaction overflows to the third-stage reactor, and the carbon dioxide sequentially react downwards.
Preferably, the carbon dioxide continuously enters the carbonization reactor, the carbon dioxide is introduced from the last stage reactor, the rest carbon dioxide overflows to the last stage reactor, and the rest carbon dioxide overflows from the first stage reactor after sequential reaction.
Preferably, the lithium hydroxide comes from a lithium hydroxide plant or from a mother liquor after lithium carbonate washing in a lithium carbonate plant; the mother liquor after the lithium carbonate washing is steam condensate or pure water.
Preferably, the centrifuged product is rinsed with pure water or with condensed water.
Preferably, the carbonization reactor is of a jacket structure, is heated by steam or cooled by circulating cooling water, and the reaction temperature is controlled between 50 and 90 ℃.
Preferably, the centrifuge is one or more of a scraper centrifuge, a belt centrifuge and a centrifuge with a back-blowing function.
Preferably, the dryer is heated with steam or with hot water or hot air.
Preferably, the carbonization reactors are connected in parallel or in series to control the desired product conversion and yield, and the reactor volume is between 5 and 50m3。
Preferably, the lithium hydroxide is refined lithium hydroxide to produce high-purity lithium carbonate; if crude lithium hydroxide is adopted, battery-grade and/or industrial-grade lithium carbonate is produced.
The invention has the beneficial effects that:
the invention adopts a multistage carbonization production process, uses carbon dioxide and feed liquid to react in a multistage reactor, can fully react the carbon dioxide and lithium hydroxide, and has high utilization rate of the carbon dioxide. The invention realizes the continuous production of lithium carbonate, and the production system has high productivity, high production efficiency, low production cost and stable product quality.
Drawings
FIG. 1 is a flow chart of a production process for producing lithium carbonate by continuous carbonization.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited to the scope of the examples. These examples are intended to illustrate the invention only and are not intended to limit the scope of the invention. In addition, various modifications may occur to those skilled in the art upon reading the present disclosure, and such equivalent variations are within the scope of the present invention as defined in the appended claims.
Example 1
(1) Putting the lithium hydroxide mother liquor into a mother liquor tank, and dissolving the lithium hydroxide mother liquor;
(2) enabling the lithium hydroxide solution in the mother liquor tank to flow into at least a 3-stage carbonization reactor, and introducing carbon dioxide into the carbonization reactor to react with lithium hydroxide;
(3) centrifugally separating the reaction product by a centrifugal machine, rinsing and centrifuging, and then connecting into a drier for heating to obtain a lithium carbonate finished product;
the carbon dioxide is converted into carbon dioxide at normal temperature and normal pressure in a low-temperature state by a vaporizer in advance, and then is introduced into a carbonization reactor;
the temperature of the gasified carbon dioxide is 0-30 ℃, the pressure is 0.1-0.5Mpa, and the flow is 0.1-1 t/h;
the lithium hydroxide is represented by Li2The O equivalent weight concentration is 10-50 g/L;
the lithium hydroxide is from a lithium hydroxide plant or from a mother liquor obtained after lithium carbonate washing in a lithium carbonate plant; the mother liquor after the lithium carbonate is washed is steam condensate or pure water;
in the carbonization reaction, the reaction temperature is between 50 and 90 ℃, and the pressure is between 0.1 and 0.5 Mpa.
Table 1 example 1 reaction Process control data
TABLE 2 Source composition of lithium hydroxide
TABLE 3 composition of carbon dioxide
| Serial number | Li2O concentration (g/L) | CO2Flow (t/h) | CO2Temperature of | CO2Pressure of | Temperature of carbonization reaction | Pressure of carbonization reaction |
| 1 | 30 | 0.1 | 10 | 0.2 | 90 | 0.1 |
| 2 | 30 | 0.5 | 10 | 0.2 | 90 | 0.1 |
| 3 | 30 | 1.0 | 10 | 0.2 | 90 | 0.1 |
In the reaction, if the refined lithium hydroxide is adopted, the high-purity lithium carbonate can be produced; if crude lithium hydroxide is used, battery-grade and technical-grade lithium carbonate can be produced.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A production method for producing multi-grade lithium carbonate by continuous carbonization is characterized by comprising the following steps:
(1) putting the lithium hydroxide mother liquor into a mother liquor tank, and dissolving the lithium hydroxide mother liquor;
(2) enabling the lithium hydroxide solution in the mother liquor tank to flow into at least a 3-stage carbonization reactor, and introducing carbon dioxide into the carbonization reactor to react with lithium hydroxide;
(3) centrifugally separating the reaction product by a centrifugal machine, rinsing and centrifuging, and then connecting into a drier for heating to obtain a lithium carbonate finished product;
the carbon dioxide is converted into carbon dioxide at normal temperature and normal pressure in a low-temperature state by a vaporizer in advance, and then is introduced into a carbonization reactor;
the temperature of the gasified carbon dioxide is 0-30 ℃, the pressure is 0.1-0.5Mpa, and the flow is 0.1-1 t/h;
the lithium hydroxide is represented by Li2The O equivalent weight concentration is 10-50 g/L;
in the carbonization reaction, the reaction temperature is between 50 and 90 ℃, and the pressure is between 0.1 and 0.5 Mpa.
2. The method for producing multi-grade lithium carbonate by continuous carbonization as claimed in claim 1, wherein: and the carbon dioxide continuously enters the carbonization reactor, the residual carbon dioxide after the first-stage reaction overflows to the second-stage reactor, and the residual carbon dioxide after the second-stage reaction overflows to the third-stage reactor and reacts downwards in sequence.
3. The method for producing multi-grade lithium carbonate by continuous carbonization as claimed in claim 1, wherein: and the carbon dioxide continuously enters the carbonization reactor, the carbon dioxide is introduced from the last stage reactor, the rest carbon dioxide overflows to the first stage reactor, and the rest carbon dioxide overflows from the first stage reactor after the sequential reaction.
4. The method for producing multi-grade lithium carbonate by continuous carbonization as claimed in claim 1, wherein: the lithium hydroxide is from a lithium hydroxide plant or from a mother liquor obtained after lithium carbonate washing in a lithium carbonate plant; the mother liquor after the lithium carbonate washing is steam condensate or pure water.
5. The method for producing multi-grade lithium carbonate by continuous carbonization as claimed in claim 1, wherein: the centrifugal separation product is rinsed with pure water or with condensed water.
6. The method for producing multi-grade lithium carbonate by continuous carbonization as claimed in claim 1, wherein: the carbonization reactor is of a jacket structure, is heated by steam or cooled by circulating cooling water, and the reaction temperature is controlled between 50 and 90 ℃.
7. The method for producing multi-grade lithium carbonate by continuous carbonization as claimed in claim 1, wherein: the centrifugal machine is one or more of a scraper centrifugal machine, a belt centrifugal machine and a centrifugal machine with a back flushing function.
8. The method for producing multi-grade lithium carbonate by continuous carbonization as claimed in claim 1, wherein: the dryer is heated by steam or hot water or hot air.
9. The method for producing multi-grade lithium carbonate by continuous carbonization as claimed in claim 1, wherein: the carbonization reactors are connected in parallel or in series so as to control the conversion rate and the yield of the required products, and the volume of the reactor is 5-50m3。
10. The method for producing multi-grade lithium carbonate by continuous carbonization as claimed in claim 1, wherein: the lithium hydroxide adopts refined lithium hydroxide to produce high-purity lithium carbonate; if crude lithium hydroxide is adopted, battery-grade and/or industrial-grade lithium carbonate is produced.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112661175A (en) * | 2021-01-21 | 2021-04-16 | 广西天源新能源材料有限公司 | Lithium carbonate preparation method based on combination of salt lake ore, lithium polymer and spodumene |
| CN115571901A (en) * | 2022-10-14 | 2023-01-06 | 西藏阿里拉果资源有限责任公司 | Method for preparing lithium carbonate by using evaporation mother liquor obtained by extracting lithium from salt lake |
| CN115849413A (en) * | 2022-12-22 | 2023-03-28 | 甘肃睿思科新材料有限公司 | Method for preparing battery-grade lithium carbonate by continuously and circularly using lithium hydroxide mother liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115571901A (en) * | 2022-10-14 | 2023-01-06 | 西藏阿里拉果资源有限责任公司 | Method for preparing lithium carbonate by using evaporation mother liquor obtained by extracting lithium from salt lake |
| CN115849413A (en) * | 2022-12-22 | 2023-03-28 | 甘肃睿思科新材料有限公司 | Method for preparing battery-grade lithium carbonate by continuously and circularly using lithium hydroxide mother liquor |
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