CN111268700A - Efficient lithium hexafluorophosphate production method - Google Patents
Efficient lithium hexafluorophosphate production method Download PDFInfo
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- CN111268700A CN111268700A CN202010156383.7A CN202010156383A CN111268700A CN 111268700 A CN111268700 A CN 111268700A CN 202010156383 A CN202010156383 A CN 202010156383A CN 111268700 A CN111268700 A CN 111268700A
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- lithium hexafluorophosphate
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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
- C01D15/005—Lithium hexafluorophosphate
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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
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Abstract
The invention discloses a high-efficiency lithium hexafluorophosphate production method, wherein phosphorus pentafluoride is buffered by a phosphorus pentafluoride buffer tank and then reacts with lithium fluoride and lithium hexafluorophosphate anhydrous hydrogen fluoride solution from a preparation tank in a synthesis kettle, after the synthetic liquid of a reaction product is pressurized, filtering to remove possible trace impurities, then feeding into a concentration kettle to distill partial hydrogen fluoride, condensing the distilled hydrogen fluoride by a condenser, collecting the hydrogen fluoride to a preparation tank, transferring to a crystallization kettle when the concentration of lithium hexafluorophosphate in the concentration kettle reaches a target value, and (3) cooling and crystallizing in a crystallization kettle, after the crystallization process is finished, feeding the lithium hexafluorophosphate anhydrous hydrogen fluoride mixture into a solid-liquid separator to perform solid-liquid separation, collecting the separated liquid into a preparation tank, feeding the separated moisture lithium hexafluorophosphate into a dryer to perform drying treatment, packaging the dried finished product, and condensing and recovering the dried tail gas, namely the anhydrous hydrogen fluoride, in a condenser. The process flow links of the invention are effectively connected, the production efficiency is high, and the product quality is stable and reliable.
Description
Technical Field
The invention relates to a method for producing lithium hexafluorophosphate.
Background
Lithium hexafluorophosphate is used as the main stream electrolyte of the lithium ion secondary battery, the production process mainly comprises a dry process and a wet process, while the anhydrous hydrogen fluoride solvent method is a wet process which is more applied in industrial production, and the problems of difficult control of the consistency of products, high energy consumption and the like mainly exist in the actual operation process.
Disclosure of Invention
The invention aims to provide a high-efficiency lithium hexafluorophosphate production method which has the advantages of effective connection of process flow links, high production efficiency and stable and reliable product quality.
The technical solution of the invention is as follows:
a high-efficiency lithium hexafluorophosphate production method is characterized in that: comprises the following steps: phosphorus pentafluoride from a front working section is buffered by a phosphorus pentafluoride buffer tank and then reacts with lithium fluoride and lithium hexafluorophosphate anhydrous hydrogen fluoride solution (the original starting is lithium fluoride anhydrous hydrogen fluoride solution) from a preparation tank in a synthesis kettle (phosphorus pentafluoride is slightly excessive to ensure that the lithium fluoride reacts sufficiently), synthetic liquid (lithium hexafluorophosphate, anhydrous hydrogen fluoride and a small amount of unreacted lithium fluoride) of a reaction product is pressurized by a synthetic liquid pump, trace impurities possibly existing in the synthetic liquid are filtered and removed by a synthetic liquid filter, then the synthetic liquid enters a concentration kettle to distill partial hydrogen fluoride, the distilled hydrogen fluoride is condensed by a condenser and then collected in the preparation tank, when the concentration of the lithium hexafluorophosphate in the concentration kettle reaches a target value, the crystallization kettle is used for cooling crystallization of the lithium hexafluorophosphate anhydrous hydrogen fluoride solution, after the crystallization procedure is finished, the lithium hexafluorophosphate anhydrous hydrogen fluoride mixture containing a certain proportion of solid particles enters a solid-liquid separator to be subjected to solid-liquid separation, and collecting the separated liquid (lithium hexafluorophosphate anhydrous hydrogen fluoride solution) to a preparation tank, sending the separated damp lithium hexafluorophosphate to a dryer for drying treatment, packaging the dried finished product, and condensing and recovering the dried tail gas-anhydrous hydrogen fluoride in a condenser.
Lithium hexafluorophosphate in the concentration kettle reaches 35-60%.
After the crystallization mother liquor is separated out by the solid-liquid separator, fresh anhydrous hydrogen fluoride is further used for cleaning lithium hexafluorophosphate solid, and the lithium hexafluorophosphate solid and the liquid separated out by the solid-liquid separator are collected to a preparation tank.
THE ADVANTAGES OF THE PRESENT INVENTION
1. Airtight connection is all realized to each relevant equipment among this lithium hexafluorophosphate apparatus for producing, makes relevant material can make full use of on the one hand, reduction in production cost, and on the other hand has effectively prevented that outside air from invading the system and toxic substance in the system from leaking, makes equipment avoid corroding, does benefit to product quality stable, makes external environment avoid polluting simultaneously.
2. The adding amount of the high-purity lithium fluoride and the fresh anhydrous hydrogen fluoride in the preparation tank is determined by calculation according to the set concentration and absolute amount of the target product lithium hexafluorophosphate in the target synthesis kettle, in the normal production process, for each batch, as the anhydrous hydrogen fluoride recovered from the concentration tank and the dryer in the preparation tank is relatively stable, the fluctuation of the concentration and the quantity of the anhydrous hydrogen fluoride solution of the lithium hexafluorophosphate obtained from the solid-liquid separator is not large, and in addition, the fresh anhydrous hydrogen fluoride cleaning liquid can be a fixed value, the feeding amount of the high-purity lithium fluoride is relatively stable, so that the stable operation of the production process is facilitated.
3. In the reaction process, the phosphorus pentafluoride is controlled to be slightly excessive, the lithium fluoride is ensured to be completely reacted, a high-precision synthetic liquid filter is subsequently arranged, and after a crystallization mother liquor is separated out by a solid-liquid separator, fresh anhydrous hydrogen fluoride is further used for cleaning lithium hexafluorophosphate solid, trace impurities possibly existing in the synthetic liquid and unreacted lithium fluoride are removed to the maximum extent, so that high-purity lithium hexafluorophosphate with the purity of more than 99.99 percent can be obtained. And simultaneously, the production system is ensured to always run in a 'clean' state.
4. Aiming at the physicochemical characteristics (low boiling point and small latent heat) of anhydrous hydrogen fluoride and the change rule of the solubility of lithium hexafluorophosphate in the anhydrous hydrogen fluoride along with the temperature (higher solubility still exists at lower temperature), a high-efficiency energy-saving lithium hexafluorophosphate crystallization mode is adopted: namely a mode of combining evaporation concentration and gradual freezing cooling crystallization. Circulating water or low-grade waste heat of the process is used as a heat source for concentration and evaporation of the concentration kettle, the concentration end point of the synthetic liquid in the concentration kettle is generally controlled to be 35-60% of the lithium hexafluorophosphate content, and the combined process of evaporation concentration and cooling crystallization is adopted, so that the defects that the quality of an evaporation concentration crystallization product is unstable when the evaporation concentration product is used independently, a small amount of residual lithium fluoride cannot be removed effectively and the like can be avoided; the method has the advantages that the independent use of cooling crystallization is avoided, the crystallization efficiency is low, a certain solid product can be obtained only when the crystallization end point temperature is low, a deep cooling unit is required to be matched, the energy efficiency is low, the energy consumption is high, the fluctuation is large, and the like; the two are organically combined, so that high-efficiency and low-consumption crystallization is realized, the product quality is stable, and the consistency is good.
5. The device has simple and efficient process flow, and small installed capacity because of no need of a matched deep cooling unit. The unit capacity occupies small area, the investment is less, and the comprehensive production cost is low.
6. The device can realize automatic and continuous production and has high intrinsic safety.
Drawings
The invention is further illustrated by the following figures and examples.
FIG. 1 is a schematic diagram of the production of lithium hexafluorophosphate used in the present invention.
Detailed Description
A high-efficiency lithium hexafluorophosphate production method comprises the following steps: phosphorus pentafluoride from a front working section is buffered by a phosphorus pentafluoride buffer tank 9 and then reacts with lithium fluoride and lithium hexafluorophosphate anhydrous hydrogen fluoride solution (the original starting is lithium fluoride anhydrous hydrogen fluoride solution) from a preparation tank 1 in a synthesis kettle 2 (phosphorus pentafluoride is slightly excessive to ensure that lithium fluoride reacts sufficiently), synthetic liquid (lithium hexafluorophosphate, anhydrous hydrogen fluoride and a small amount of unreacted lithium fluoride) of a reaction product is pressurized by a synthetic liquid pump 3, trace impurities possibly existing in the synthetic liquid are filtered and removed by a synthetic liquid filter 4, then the synthetic liquid enters a concentration kettle 5 to distill partial hydrogen fluoride, the distilled hydrogen fluoride is condensed by a condenser 6 and then collected in the preparation tank 1, when the concentration of the lithium hexafluorophosphate in the concentration kettle reaches a target value, the crystallization kettle 7 is used for cooling and crystallizing lithium hexafluorophosphate anhydrous hydrogen fluoride solution in the crystallization kettle 7, after a crystallization program is finished, the lithium hexafluorophosphate anhydrous hydrogen fluoride mixture containing a certain proportion of solid particles enters a solid-liquid separator 8 to implement solid-liquid separation Liquid separation, collecting the separated liquid (lithium hexafluorophosphate anhydrous hydrogen fluoride solution) to a preparation tank 1, sending the separated damp lithium hexafluorophosphate to a dryer 10 for drying treatment, packaging the dried finished product, and condensing and recovering the dried tail gas-anhydrous hydrogen fluoride in a condenser 6.
The concentration of lithium hexafluorophosphate in the concentration kettle reaches a target value of 35-60%.
After the crystallization mother liquor is separated out by the solid-liquid separator, fresh anhydrous hydrogen fluoride is further used for cleaning lithium hexafluorophosphate solid, and the lithium hexafluorophosphate solid and the liquid separated out by the solid-liquid separator are collected to a preparation tank.
Claims (3)
1. A high-efficiency lithium hexafluorophosphate production method is characterized in that: comprises the following steps: phosphorus pentafluoride from a front working section reacts with lithium fluoride and lithium hexafluorophosphate anhydrous hydrogen fluoride solution from a preparation tank (1) in a synthesis kettle (2) after being buffered by a phosphorus pentafluoride buffer tank (9), reaction product synthetic liquid is pressurized by a synthetic liquid pump (3), a synthetic liquid filter (4) is used for filtering to remove possible trace impurities, then the synthetic liquid enters a concentration kettle (5) for distilling part of hydrogen fluoride, the evaporated hydrogen fluoride is condensed by a condenser (6) and then collected in the preparation tank (1), when the concentration of the lithium hexafluorophosphate in the concentration kettle reaches a target value, the synthetic liquid is transferred to a crystallization kettle (7), the lithium hexafluorophosphate anhydrous hydrogen fluoride solution is cooled and crystallized in the crystallization kettle (7), after the crystallization procedure is finished, the lithium hexafluorophosphate anhydrous hydrogen fluoride mixture containing a certain proportion of solid particles enters a solid-liquid separator (8) for solid-liquid separation, the separated liquid is collected in the preparation tank (1), and (3) conveying the separated damp lithium hexafluorophosphate product to a dryer (10) for drying treatment, packaging the dried finished product, and condensing and recovering the dried tail gas, namely the anhydrous hydrogen fluoride in a condenser (6).
2. The method for producing high-efficiency lithium hexafluorophosphate according to claim 1, wherein the method comprises the following steps: the lithium hexafluorophosphate content in the concentration kettle reaches 35-60%.
3. The method for producing high-efficiency lithium hexafluorophosphate according to claim 1 or 2, wherein: after the crystallization mother liquor is separated out by the solid-liquid separator, fresh anhydrous hydrogen fluoride is further used for cleaning lithium hexafluorophosphate solid, and the lithium hexafluorophosphate solid and the liquid separated out by the solid-liquid separator are collected to a preparation tank.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321228A (en) * | 2021-06-11 | 2021-08-31 | 厚成科技（南通）有限公司 | Lithium hexafluorophosphate purification method |
| CN114713154A (en) * | 2022-04-30 | 2022-07-08 | 南京佳华工程技术有限公司 | System and process method for preparing lithium hexafluorophosphate |
| CN115744938A (en) * | 2022-11-14 | 2023-03-07 | 万华化学集团股份有限公司 | Method for preparing spherical lithium hexafluorophosphate crystal |
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| CN101544361A (en) * | 2009-05-07 | 2009-09-30 | 洛阳森蓝化工材料科技有限公司 | Process and device for continuous preparation of lithium hexafluorophosphate |
| CN101605723A (en) * | 2007-02-08 | 2009-12-16 | 斯泰拉化工公司 | The manufacture method of hexafluorophosphate |
| CN106882819A (en) * | 2017-03-29 | 2017-06-23 | 东营石大胜华新能源有限公司 | A kind of lithium hexafluoro phosphate prepares purification process |
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2020
- 2020-03-09 CN CN202010156383.7A patent/CN111268700A/en active Pending
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| CN101605723A (en) * | 2007-02-08 | 2009-12-16 | 斯泰拉化工公司 | The manufacture method of hexafluorophosphate |
| CN101544361A (en) * | 2009-05-07 | 2009-09-30 | 洛阳森蓝化工材料科技有限公司 | Process and device for continuous preparation of lithium hexafluorophosphate |
| CN106882819A (en) * | 2017-03-29 | 2017-06-23 | 东营石大胜华新能源有限公司 | A kind of lithium hexafluoro phosphate prepares purification process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321228A (en) * | 2021-06-11 | 2021-08-31 | 厚成科技（南通）有限公司 | Lithium hexafluorophosphate purification method |
| CN114713154A (en) * | 2022-04-30 | 2022-07-08 | 南京佳华工程技术有限公司 | System and process method for preparing lithium hexafluorophosphate |
| CN114713154B (en) * | 2022-04-30 | 2022-12-16 | 南京佳华工程技术有限公司 | System and process method for preparing lithium hexafluorophosphate |
| CN115744938A (en) * | 2022-11-14 | 2023-03-07 | 万华化学集团股份有限公司 | Method for preparing spherical lithium hexafluorophosphate crystal |
| CN115744938B (en) * | 2022-11-14 | 2024-04-09 | 万华化学集团股份有限公司 | Method for preparing spherical lithium hexafluorophosphate crystal |
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Application publication date: 20200612 |