CN110668472A - Method and device for crystallizing lithium hexafluorophosphate synthesis mother liquor - Google Patents
Method and device for crystallizing lithium hexafluorophosphate synthesis mother liquor Download PDFInfo
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- CN110668472A CN110668472A CN201911087993.XA CN201911087993A CN110668472A CN 110668472 A CN110668472 A CN 110668472A CN 201911087993 A CN201911087993 A CN 201911087993A CN 110668472 A CN110668472 A CN 110668472A
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- C01D15/00—Lithium compounds
- C01D15/005—Lithium hexafluorophosphate
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Abstract
The invention provides a method and a device for crystallizing lithium hexafluorophosphate synthetic mother liquor, belonging to the technical field of lithium hexafluorophosphate preparation. The crystallization device comprises a mother liquor tank for storing synthetic mother liquor; the crystallizer is used for carrying out freezing crystallization and filtration on the synthetic mother liquor in the mother liquor tank to obtain lithium hexafluorophosphate, and drying the lithium hexafluorophosphate; the evaporation concentrator is used for carrying out evaporation concentration on the mother liquor after crystallization and filtration and separating hydrofluoric acid gas; and the compression condenser is used for compressing and condensing the hydrofluoric acid gas separated from the evaporation concentrator to obtain hydrofluoric acid liquid. The invention firstly freezes and crystallizes the synthetic mother liquor, then evaporates and crystallizes the synthetic mother liquor, and concentrates the synthetic mother liquor in an unsaturated solution state, thereby solving the defects of easy entrainment of HF and low product quality in the product in the prior art.
Description
Technical Field
The invention belongs to the technical field of lithium hexafluorophosphate preparation, and particularly relates to a method for crystallizing a lithium hexafluorophosphate synthetic liquid.
Background
Lithium hexafluorophosphate is used as lithium ion battery electrolyte, is mainly used in the fields of lithium ion power batteries, lithium ion energy storage batteries and other daily batteries, and has become the lithium ion battery electrolyte which cannot be replaced at present. At present, a hydrogen fluoride solvent method is mainly adopted for synthesizing lithium hexafluorophosphate, a static cooling crystallization method is adopted for synthetic liquid, the synthetic liquid is reduced to minus 60 ℃ through a certain temperature gradient, and the static crystallization is frozen for 20 to 40 hours, so that special cryogenic equipment is needed, the power consumption is high, and the cryogenic energy efficiency at minus 60 ℃ is lower.
In order to solve the above problems, the prior art (CN107244681B) discloses a method and an apparatus for continuously preparing lithium hexafluorophosphate, wherein a synthesis solution is heated by a heater and then enters a continuous evaporation crystallizer, the materials in the crystallization are stirred under vacuum, the obtained crystals are left in an elutriation leg and discharged by an external pump for separation and drying, and the separated mother liquor is pumped back to the crystallizer for recycling; and part of anhydrous hydrogen fluoride evaporated from the continuous evaporation crystallizer is discharged from the top of the crystallizer and condensed into liquid hydrogen fluoride for recycling. The prior art adopts an evaporative crystallization process, does not need cryogenic equipment, and greatly reduces energy consumption.
Because the crystallization speed of lithium hexafluorophosphate has great influence on the product quality, the crystallization speed is too high at high temperature, and a lot of HF is carried in the crystal after the crystal passes, so that the HF exceeds the standard and is difficult to handle. Therefore, in the prior art, the synthesis solution is heated to 45-50 ℃ and then enters the evaporative crystallizer for crystallization, namely, the saturated lithium hexafluorophosphate solution is heated, the heating temperature exceeds the boiling point of HF, and the crystallization is easy to clamp the HF, so that the product quality is influenced.
Disclosure of Invention
Based on the background problem, the invention aims to provide a method for crystallizing lithium hexafluorophosphate synthetic liquid, which comprises the steps of crystallizing the synthetic liquid in a refrigerant at the temperature of-20 to-30 ℃, and then evaporating and concentrating crystallized mother liquor, namely concentrating the mother liquor in an unsaturated solution state, so that the defects of easy entrainment of HF and low product quality in the prior art are overcome; another object of the present invention is to provide an apparatus for carrying out the above method for crystallizing a lithium hexafluorophosphate synthetic liquid and a mother liquor.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
the lithium hexafluorophosphate synthesis mother liquor crystallization method comprises the steps of freezing and crystallizing synthesis mother liquor in a refrigerant to obtain lithium hexafluorophosphate, evaporating and concentrating the mother liquor after crystallization and filtration, and returning the concentrated mother liquor to be mixed with the synthesis mother liquor for crystallization.
Wherein, the lithium hexafluorophosphate obtained in the crystallization process is dried at the temperature of 30-70 ℃ for 2-4 h.
In one embodiment, the temperature of the refrigerant in the crystallization process is-20 to-30 ℃, and the freezing time is 4 to 6 hours.
Wherein the concentration of lithium hexafluorophosphate in the mother liquor after crystallization and filtration and the concentration of lithium hexafluorophosphate in the synthetic liquor are 0.5-0.75: 1.
In one embodiment, the temperature of the evaporation concentration process is 30-70 ℃.
Wherein the concentration ratio of lithium hexafluorophosphate in the mother liquor after evaporation and concentration to lithium hexafluorophosphate in the mother liquor after crystallization and filtration is 1.3-1.7: 1.
In one embodiment, the vapor phase hydrofluoric acid evaporated by the evaporation concentration process forms liquid phase hydrofluoric acid through the compression condensation process, and returns to the synthesis process for reuse.
Wherein the pressure of the compression process is 0.2-2MPa, and the condensation temperature is-20 to-30 ℃.
In order to achieve the above object, the present invention also provides an apparatus for crystallizing a lithium hexafluorophosphate synthesis mother liquor, comprising: the mother liquor tank is used for storing the synthetic liquor and the crystallized filtered mother liquor; the crystallizer is used for carrying out freezing crystallization, filtration and drying on the synthetic mother liquor in the mother liquor tank to obtain lithium hexafluorophosphate; the evaporation concentrator is used for carrying out evaporation concentration on the mother liquor after crystallization and filtration and separating hydrofluoric acid gas; and the compression condenser is used for compressing and condensing the hydrofluoric acid gas separated from the evaporation concentrator to obtain hydrofluoric acid liquid.
Preferably, a stirring component is arranged in the mother liquid tank, and the crystallizer is a dynamic crystallizer with a stirring component.
Compared with the prior art, the invention has the following effects:
1. the invention adopts the method of freezing, crystallizing and evaporating the synthetic mother liquor for crystallization, and the synthetic mother liquor is concentrated in the state of non-saturated solution, thereby overcoming the defects of easy HF entrainment and low product quality in the prior art and improving the crystallization effect.
2. The mother liquor after crystallization and concentration is directly used for the crystallization process without returning to the synthesis process, so that the capacity and the efficiency of the synthesis process are improved, the overall production efficiency is improved by more than 30%, the energy consumption is reduced by 35%, the HF consumption is reduced by 15%, and the production cost is reduced by 10%.
3. The invention carries out freezing crystallization in a temperature range of-20 to-30 ℃, the crystallization temperature zone is relatively higher, deep cooling equipment is not needed, the conventional refrigerator can work in a high-efficiency range, the efficiency is high, and the energy consumption is reduced.
4. The crystallizer in the crystallization device adopts a dynamic crystallizer with a stirring function, the grain size of the crystallized crystal can be controlled in a certain range, and the crystallizer is of an integrated structure of crystallization, filtration and drying, so that the working efficiency is high.
Drawings
Fig. 1 is a schematic view of a lithium hexafluorophosphate synthesis mother liquor crystallization apparatus in embodiment 1 of the present invention.
Detailed Description
The method mainly aims to solve the defects in the prior art, the synthesis mother liquor is frozen and crystallized in a refrigerant to obtain lithium hexafluorophosphate, the crystallized mother liquor is evaporated and concentrated, and the concentrated mother liquor is returned to be mixed with the synthesis mother liquor for crystallization. Is beneficial to improving the crystallization efficiency.
The present invention will be described in detail with reference to specific examples.
Example 1
In this embodiment, there is provided a lithium hexafluorophosphate synthesis mother liquor crystallization apparatus, as shown in fig. 1, including: mother liquor tank 1, crystallizer 2, evaporation concentrator 3, compressor 4 and condenser 5, mother liquor tank 1 are used for depositing the synthetic mother liquor of synthesis technology output, and the synthetic mother liquor is the hydrogen fluoride mother liquor that contains lithium hexafluorophosphate, for the homogeneity of guaranteeing the synthetic mother liquor of mother liquor tank 1, be equipped with the stirring subassembly in the mother liquor tank 1 for stir synthetic mother liquor in succession. The synthetic mother liquor in the mother liquor tank 1 is conveyed to the crystallizer 2 through a conveying pump.
The crystallizer 2 is used for freezing and crystallizing mother liquor, the crystallizer 2 is also provided with a stirring component, the grain size of crystallized crystals can be controlled within a certain range, and lithium hexafluorophosphate can be obtained by filtering after crystallization. The crystallizer of the embodiment is an integrated device of crystallization, filtration and drying, the crystallized mother liquor is output to the evaporation concentrator 3 after crystallization, lithium hexafluorophosphate is left in the crystallizer 2, and then dry nitrogen is introduced into the crystallizer 2 to dry the lithium hexafluorophosphate. It should be noted that the structure of the crystallizer 2 is not limited to this, and in other embodiments, the crystallization, filtration, and drying may be separated, that is, one crystallization device, one filtration device, and one drying device are provided. The bottom of the crystallizer 2 is communicated with the evaporation concentrator 3 through a pipeline so as to convey the crystallized mother liquor into the evaporation concentrator 3 for evaporation concentration.
The evaporation concentrator 3 is used for evaporating and concentrating the mother liquor after crystallization and filtration conveyed in the crystallizer 2, the evaporation concentrator 3 is heated by adopting an outer jacket, hot water is filled in the outer jacket, and the bottom of the evaporation concentrator 3 is communicated with the mother liquor tank 1 through a pipeline so as to return the concentrated mother liquor into the mother liquor tank 1 through the pipeline for recrystallization.
Hydrofluoric acid gas can spill over from the top of the evaporation concentrator 3 in the evaporation concentration process, in order to recycle the hydrofluoric acid gas, the top of the evaporation concentrator 3 is sequentially communicated with a compressor 4 and a condenser 5 through pipelines, and the hydrofluoric acid gas is compressed by the compressor and then enters the condenser to be condensed to obtain hydrofluoric acid liquid.
It should be noted that the crystallizer 2, the evaporator-concentrator 3, the compressor 4 and the condenser 5 used in this embodiment are conventional devices in the art, and the structure thereof will not be described again.
Example 2
In this example, 200kg of a hydrogen fluoride mother liquor from a synthesis process was introduced into a mother liquor tank 1 by using the processing apparatus in example 1, and the mass concentration of lithium hexafluorophosphate in the hydrogen fluoride mother liquor was 20%, and the stirring was continuously carried out by turning on a stirring means.
The mother liquor is conveyed into a crystallizer 2 through a conveying pump, lithium hexafluorophosphate at the crystallization position is frozen for 6 hours through a refrigerant with the temperature of minus 20 ℃, the freezing temperature and the freezing time have certain influence on crystallization, and a product with better shape and quality can be obtained according to a temperature-time crystallization curve. And drying the filtered product by using dry nitrogen, controlling the drying temperature to be 30-40 ℃, the drying time to be 4 hours, obtaining 48kg of dried lithium hexafluorophosphate, determining that the content of HF in the lithium hexafluorophosphate is less than 10ppm, and transferring the product to a product packaging process to package the product, wherein the dried product is qualified.
The mass concentration of lithium hexafluorophosphate in the filtered mother liquor of the crystals obtained from the crystallizer 2 is 13%, the filtered mother liquor of the crystals is conveyed to an evaporation concentrator 3, the water temperature in an outer jacket is controlled at 30 ℃, and the crystallized mother liquor is concentrated into a concentrated mother liquor with the mass concentration of lithium hexafluorophosphate of 22.1%.
The evaporation concentrator 3 can overflow gas-phase hydrofluoric acid in the evaporation process, the overflowing hydrofluoric acid gas is compressed to 0.3MPa through the acid-resistant compressor 4, the compressed gas enters the condenser 5, the temperature of a refrigerant in the condenser 5 is controlled to be-30 ℃, the hydrofluoric acid gas is condensed into hydrofluoric acid liquid, and the obtained liquid hydrofluoric acid is returned to the synthesis process for reuse, and more than 98% of the hydrofluoric acid can be recovered by the method.
Example 3
Example 3 differs from example 2 in that: controlling the temperature of a refrigerant in the crystallizer 2 to be-30 ℃ and the freezing time to be 6 h; the drying temperature is 70 ℃, the drying time is 2 hours, and the mass concentration of lithium hexafluorophosphate in the crystallized mother liquor obtained from the crystallizer 2 is 10 percent; conveying the crystallized mother liquor to an evaporation concentrator 3, and controlling the mass concentration of lithium hexafluorophosphate in the concentrated mother liquor to be 15%; the pressure of the compressed gas phase hydrofluoric acid is 2MPa, and the condensing temperature is-20 ℃.
Example 4
Example 4 differs from example 2 in that: controlling the temperature of a refrigerant in the crystallizer 2 to be-20 ℃, the freezing time to be 4 hours, the drying temperature to be 50 ℃, and the drying time to be 3 hours, wherein the mass concentration of lithium hexafluorophosphate in the crystallized mother liquor obtained from the crystallizer 2 is 15 percent; conveying the crystallized mother liquor to an evaporation concentrator 3, and controlling the mass concentration of lithium hexafluorophosphate in the concentrated mother liquor to be 19.5%; the pressure of the compressed gas phase hydrofluoric acid is 1MPa, and the condensing temperature is-25 ℃.
It should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications belong to the protection scope of the present invention.
Claims (10)
1. The method for crystallizing the lithium hexafluorophosphate synthetic mother liquor is characterized in that the synthetic mother liquor is frozen and crystallized in a refrigerant to obtain the lithium hexafluorophosphate, the mother liquor after crystallization and filtration is evaporated and concentrated, and the concentrated mother liquor is returned to be mixed with the synthetic mother liquor for crystallization.
2. The method for crystallizing lithium hexafluorophosphate synthesis mother liquor as claimed in claim 1, wherein the lithium hexafluorophosphate obtained in the crystallization process is dried at 30-70 ℃ for 2-4 hours.
3. The crystallization method of lithium hexafluorophosphate synthetic liquid according to claim 1, wherein the temperature of refrigerant in the crystallization process is-20 to-30 ℃ and the freezing time is 4 to 6 hours.
4. The method for crystallizing lithium hexafluorophosphate synthesis mother liquor according to claim 3, wherein the concentration ratio of lithium hexafluorophosphate in the mother liquor after the crystallization filtration to lithium hexafluorophosphate in the synthesis mother liquor is 0.5 to 0.75: 1.
5. The method for crystallizing lithium hexafluorophosphate synthesis mother liquor as claimed in claim 1, wherein the temperature of the evaporation concentration process is 30 to 70 ℃.
6. The method for crystallizing lithium hexafluorophosphate synthesis mother liquor as claimed in claim 5, wherein the concentration ratio of lithium hexafluorophosphate in the mother liquor after evaporation concentration to lithium hexafluorophosphate in the mother liquor after crystal filtration is 1.3 to 1.7: 1.
7. The method for crystallizing lithium hexafluorophosphate synthesis mother liquor as claimed in claim 1, wherein the vapor phase hydrofluoric acid evaporated by the evaporation and concentration process is formed into liquid phase hydrofluoric acid by the compression and condensation process and returned to the synthesis process for reuse.
8. The crystallization method of lithium hexafluorophosphate synthesis mother liquor as claimed in claim 7, wherein the pressure of the compression process is 0.2-2MPa, and the condensation temperature is-20 to-30 ℃.
9. Lithium hexafluorophosphate synthesis mother liquor crystallization device, its characterized in that includes:
the mother liquor tank is used for storing the synthetic liquor and the crystallized filtered mother liquor;
the crystallizer is used for carrying out freezing crystallization, filtration and drying on the synthetic mother liquor in the mother liquor tank to obtain lithium hexafluorophosphate;
the evaporation concentrator is used for carrying out evaporation concentration on the mother liquor after crystallization and filtration and separating hydrofluoric acid gas;
and the compression condenser is used for compressing and condensing the hydrofluoric acid gas separated from the evaporation concentrator to obtain hydrofluoric acid liquid.
10. The apparatus for crystallizing lithium hexafluorophosphate synthesis mother liquor as claimed in claim 9, wherein a stirring assembly is provided in said mother liquor tank, and said crystallizer is a dynamic crystallizer with a stirring assembly.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114788961A (en) * | 2022-05-09 | 2022-07-26 | 西安航天华威化工生物工程有限公司 | Continuous dynamic crystallization process device and method for high-purity lithium hexafluorophosphate |
| CN116135786A (en) * | 2021-11-18 | 2023-05-19 | 杉杉新材料（衢州）有限公司 | Preparation method of lithium hexafluorophosphate crystals with uniform particle size |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110097626A1 (en) * | 2008-08-08 | 2011-04-28 | Stella Chemifa Corporation | Process for production hexafluorophosphates |
| KR101223384B1 (en) * | 2012-06-01 | 2013-01-16 | 오씨아이머티리얼즈 주식회사 | Apparatus and method for manufacturing lithium hexafluoro phosphate |
| US20130143112A1 (en) * | 2010-08-17 | 2013-06-06 | Central Glass Company, Limited | Method for Producing a Lithium Hexafluorophosphate Concentrated Liquid |
| CN205307856U (en) * | 2015-10-29 | 2016-06-15 | 湖北省宏源药业科技股份有限公司 | LiPF6 heavy crystal device |
| 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 |
| CN107244681A (en) * | 2017-03-29 | 2017-10-13 | 东营石大胜华新能源有限公司 | A kind of continuous method and apparatus for preparing lithium hexafluoro phosphate |
| CN110182828A (en) * | 2019-06-14 | 2019-08-30 | 江苏新泰材料科技有限公司 | A kind of lithium hexafluoro phosphate dynamic crystallization device and method for crystallising |
-
2019
- 2019-11-08 CN CN201911087993.XA patent/CN110668472A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110097626A1 (en) * | 2008-08-08 | 2011-04-28 | Stella Chemifa Corporation | Process for production hexafluorophosphates |
| US20130143112A1 (en) * | 2010-08-17 | 2013-06-06 | Central Glass Company, Limited | Method for Producing a Lithium Hexafluorophosphate Concentrated Liquid |
| KR101223384B1 (en) * | 2012-06-01 | 2013-01-16 | 오씨아이머티리얼즈 주식회사 | Apparatus and method for manufacturing lithium hexafluoro phosphate |
| CN205307856U (en) * | 2015-10-29 | 2016-06-15 | 湖北省宏源药业科技股份有限公司 | LiPF6 heavy crystal device |
| 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 |
| CN107244681A (en) * | 2017-03-29 | 2017-10-13 | 东营石大胜华新能源有限公司 | A kind of continuous method and apparatus for preparing lithium hexafluoro phosphate |
| CN110182828A (en) * | 2019-06-14 | 2019-08-30 | 江苏新泰材料科技有限公司 | A kind of lithium hexafluoro phosphate dynamic crystallization device and method for crystallising |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116135786A (en) * | 2021-11-18 | 2023-05-19 | 杉杉新材料（衢州）有限公司 | Preparation method of lithium hexafluorophosphate crystals with uniform particle size |
| CN114788961A (en) * | 2022-05-09 | 2022-07-26 | 西安航天华威化工生物工程有限公司 | Continuous dynamic crystallization process device and method for high-purity lithium hexafluorophosphate |
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