CN111994924A - Novel method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as raw material - Google Patents
Novel method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as raw material Download PDFInfo
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- CN111994924A CN111994924A CN202010938222.3A CN202010938222A CN111994924A CN 111994924 A CN111994924 A CN 111994924A CN 202010938222 A CN202010938222 A CN 202010938222A CN 111994924 A CN111994924 A CN 111994924A
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- lithium fluoride
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- lithium carbonate
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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
- C01D15/04—Halides
Abstract
The invention relates to a novel method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as a raw material. And adding hydrofluoric acid into the solution to directly precipitate the lithium fluoride, and filtering, washing and drying to obtain the high-purity lithium fluoride. Compared with the traditional method of obtaining high-purity lithium carbonate by cracking and then reacting with hydrofluoric acid to obtain high-purity lithium fluoride, the method greatly improves the direct yield of the product, reduces the production cost and is worth popularizing.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a novel method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as a raw material.
Background
Lithium fluoride is one of necessary raw materials for producing commonly used electrolyte lithium hexafluorophosphate of the ion battery, the production method of the battery grade lithium fluoride is a cracking method at present, but the production cost of the cracking method is higher, and the direct yield of lithium carbonate in the reaction process is relatively lower.
Disclosure of Invention
In view of this, a new method for producing high-purity lithium fluoride by using industrial-grade lithium carbonate as a raw material with high direct yield and low production cost is provided. Which comprises the following steps of; the method comprises the following steps:
(1) slurrying lithium carbonate with pure water, feeding the slurry into a carbonic acid hydrogenation tower, introducing carbon dioxide for carbonic acid hydrogenation, and filtering after the carbonic acid hydrogenation is finished to obtain a lithium bicarbonate solution, wherein the chemical reaction equation is as follows:
the reaction is carried out for 120min at the temperature of 20-30 ℃, and the solution is filtered to obtain a lithium bicarbonate solution after the reaction is finished;
(2) removing impurities by ion exchange to obtain a high-purity lithium bicarbonate solution;
(3) adding hydrofluoric acid into the solution to directly precipitate lithium fluoride, filtering, washing and drying to obtain high-purity lithium fluoride, wherein the chemical reaction equation is as follows:
further, the mother liquor is neutralized to PH = 7-8 by adding alkali, and is subjected to fluorine removal by using aluminum sulfate, filtration and discharge.
Further, the direct extraction rate of the lithium bicarbonate obtained in the step (1) reaches 97%.
Further, the reaction environment in the step (3) is normal temperature and normal pressure.
Compared with the prior art, the method has the advantages that compared with the traditional method that high-purity lithium carbonate is obtained through cracking and then reacts with hydrofluoric acid to obtain high-purity lithium fluoride, the method greatly improves the direct yield of the product and reduces the production cost.
Drawings
Fig. 1 is a process flow chart of a new method for producing high-purity lithium fluoride by using industrial-grade lithium carbonate as a raw material in an embodiment of the invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and the accompanying drawings.
Referring to fig. 1, a new process for producing high purity lithium fluoride from industrial grade lithium carbonate is shown, according to an embodiment of the present invention, comprising the steps of:
(1) slurrying lithium carbonate with pure water, feeding the slurry into a carbonic acid hydrogenation tower, introducing carbon dioxide for carbonic acid hydrogenation, and filtering after the carbonic acid hydrogenation is finished to obtain a lithium bicarbonate solution, wherein the chemical reaction equation is as follows:
the reaction is carried out for 120min at the temperature of 20-30 ℃, and the solution is filtered to obtain a lithium bicarbonate solution after the reaction is finished;
(2) removing impurities by ion exchange to obtain a high-purity lithium bicarbonate solution;
(3) adding hydrofluoric acid into the solution to directly precipitate lithium fluoride, filtering, washing and drying to obtain high-purity lithium fluoride, wherein the chemical reaction equation is as follows:
further, as a preferable mode of the embodiment, the mother liquor is neutralized to pH = 7-8 by adding alkali, and is subjected to fluorine removal by using aluminum sulfate, and is discharged after being filtered.
Further, as a preferable example of the present embodiment, the lithium bicarbonate extraction rate in the step (1) is 97%.
Further, in this embodiment, it is preferable that the reaction environment in the step (3) is normal temperature and normal pressure.
Further, as the optimization of the embodiment, the production cost of the new method and the production cost of the traditional method sharing the flow are eliminated, the new method reduces the cost of cracking and lithium (2 g/l) contained in the mother liquor, and the cost of 6000 yuan RMB can be saved by measuring and calculating each ton of lithium fluoride.
The above disclosure is only one preferred embodiment of the present invention, and certainly should not be construed as limiting the scope of the invention, which is defined by the claims and their equivalents.
Claims (4)
1. A new method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as a raw material is characterized by comprising the following steps: the method comprises the following steps:
(1) slurrying lithium carbonate with pure water, feeding the slurry into a carbonic acid hydrogenation tower, introducing carbon dioxide for carbonic acid hydrogenation, and filtering after the carbonic acid hydrogenation is finished to obtain a lithium bicarbonate solution, wherein the chemical reaction equation is as follows:
the reaction is carried out for 120min at the temperature of 20-30 ℃, and the solution is filtered to obtain a lithium bicarbonate solution after the reaction is finished;
(2) removing impurities by ion exchange to obtain a high-purity lithium bicarbonate solution;
(3) adding hydrofluoric acid into the solution to directly precipitate lithium fluoride, filtering, washing and drying to obtain high-purity lithium fluoride, wherein the chemical reaction equation is as follows:
2. the novel process for producing high purity lithium fluoride from technical grade lithium carbonate as claimed in claim 1, wherein: and (3) adding alkali into the mother liquor to neutralize the mother liquor until the pH = 7-8, removing fluorine by using aluminum sulfate, filtering and discharging.
3. The novel process for producing high purity lithium fluoride from technical grade lithium carbonate as claimed in claim 1, wherein: the direct extraction rate of the lithium bicarbonate obtained in the step (1) reaches 97%.
4. The novel process for producing high purity lithium fluoride from technical grade lithium carbonate as claimed in claim 1, wherein: and (3) the reaction environment in the step (3) is normal temperature and normal pressure.
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| CN202010938222.3A CN111994924A (en) | 2020-09-09 | 2020-09-09 | Novel method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as raw material |
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| CN202010938222.3A CN111994924A (en) | 2020-09-09 | 2020-09-09 | Novel method for producing high-purity lithium fluoride by taking industrial-grade lithium carbonate as raw material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112678849A (en) * | 2021-01-04 | 2021-04-20 | 江西云锂材料股份有限公司 | Method for preparing high-purity lithium carbonate by using lithium hydroxide |
| CN114538481A (en) * | 2022-03-29 | 2022-05-27 | 江西飞宇新能源科技有限公司 | Technical method for preparing lithium fluoride from industrial-grade lithium carbonate |
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| RU2006107861A (en) * | 2006-03-13 | 2007-09-20 | Открытое акционерное общество "Новосибирский завод химконцентратов" (RU) | METHOD FOR PRODUCING HIGH PURE LITHIUM FLUORIDE |
| CN101723414A (en) * | 2009-12-11 | 2010-06-09 | 多氟多化工股份有限公司 | Method for producing battery-grade lithium fluoride |
| CN101723415A (en) * | 2010-02-04 | 2010-06-09 | 江西东鹏新材料有限责任公司 | Novel process for producing cell-grade lithium fluoride |
| CN106315629A (en) * | 2016-08-30 | 2017-01-11 | 山东瑞福锂业有限公司 | Technology for preparing high-purity lithium carbonate through recovering of battery-grade lithium carbonate lithium precipitation mother liquor |
| CN111559750A (en) * | 2020-03-27 | 2020-08-21 | 白银中天化工有限责任公司 | Efficient continuous electronic-grade lithium fluoride production process |
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2020
- 2020-09-09 CN CN202010938222.3A patent/CN111994924A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2006107861A (en) * | 2006-03-13 | 2007-09-20 | Открытое акционерное общество "Новосибирский завод химконцентратов" (RU) | METHOD FOR PRODUCING HIGH PURE LITHIUM FLUORIDE |
| CN101723414A (en) * | 2009-12-11 | 2010-06-09 | 多氟多化工股份有限公司 | Method for producing battery-grade lithium fluoride |
| CN101723415A (en) * | 2010-02-04 | 2010-06-09 | 江西东鹏新材料有限责任公司 | Novel process for producing cell-grade lithium fluoride |
| CN106315629A (en) * | 2016-08-30 | 2017-01-11 | 山东瑞福锂业有限公司 | Technology for preparing high-purity lithium carbonate through recovering of battery-grade lithium carbonate lithium precipitation mother liquor |
| CN111559750A (en) * | 2020-03-27 | 2020-08-21 | 白银中天化工有限责任公司 | Efficient continuous electronic-grade lithium fluoride production process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112678849A (en) * | 2021-01-04 | 2021-04-20 | 江西云锂材料股份有限公司 | Method for preparing high-purity lithium carbonate by using lithium hydroxide |
| CN114538481A (en) * | 2022-03-29 | 2022-05-27 | 江西飞宇新能源科技有限公司 | Technical method for preparing lithium fluoride from industrial-grade lithium carbonate |
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Application publication date: 20201127 |