CN110937587A - Method and device for preparing lithium hexafluorophosphate by adopting microreactor - Google Patents
Method and device for preparing lithium hexafluorophosphate by adopting microreactor Download PDFInfo
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- CN110937587A CN110937587A CN201911394711.0A CN201911394711A CN110937587A CN 110937587 A CN110937587 A CN 110937587A CN 201911394711 A CN201911394711 A CN 201911394711A CN 110937587 A CN110937587 A CN 110937587A
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- microreactor
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- 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
Abstract
The invention provides a method and a device for preparing lithium hexafluorophosphate by adopting a microreactor, belonging to the technical field of synthesis of lithium hexafluorophosphate. The synthesizing device comprises: the first microreactor is used for reacting chlorine with phosphorus trichloride to synthesize phosphorus pentachloride; and the second microreactor is used for reacting phosphorus pentachloride. The invention adopts the microreactor to carry out chlorination and fluorination reactions, has high intermolecular heat transfer and mass transfer efficiency of reaction materials, improves the reaction efficiency, and can lead out reaction heat, thereby ensuring the safety.
Description
Technical Field
The invention belongs to the technical field of preparation of lithium hexafluorophosphate, and particularly relates to a method for preparing lithium hexafluorophosphate by adopting a microreactor.
Background
Lithium hexafluorophosphate (LiPF)6) The 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 an irreplaceable lithium ion battery electrolyte at present.
At present, a hydrogen fluoride solvent method is mainly adopted for synthesizing lithium hexafluorophosphate, namely phosphorus pentafluoride and lithium fluoride are adopted to react in a hydrogen fluoride solvent to generate lithium hexafluorophosphate; lithium hexafluorophosphate may be synthesized by using chlorine gas, phosphorus trichloride, lithium chloride, hydrogen fluoride, etc. as raw materials, but the above synthesis process is very dangerous because the chlorination reaction of chlorine gas and phosphorus trichloride and the reaction of hydrogen fluoride and phosphorus pentachloride are very violent and the heat is strongly released during the reaction, as disclosed in the prior art (CN 103069638A).
Disclosure of Invention
Based on the background problem, the invention aims to provide a method for preparing lithium hexafluorophosphate by using a microreactor, wherein the microreactor is used for chlorination and fluorination reaction, the intermolecular heat transfer and mass transfer efficiency of reaction materials is high, the reaction efficiency is improved, and reaction heat can be led out, so that the safety is guaranteed; another object of the present invention is to provide an apparatus for preparing lithium hexafluorophosphate using a microreactor.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a method for preparing lithium hexafluorophosphate by using a microreactor is characterized in that chlorine, phosphorus trichloride, hydrogen fluoride and a lithium fluoride solution are introduced into the microreactor to react so as to realize instant uniform mixing and rapid reaction of materials and to lead out reaction heat.
In one embodiment, chlorine and phosphorus trichloride are introduced into a first microreactor to react to synthesize phosphorus pentachloride gas; introducing anhydrous hydrogen fluoride and phosphorus pentachloride gas synthesized in the first microreactor into a second microreactor to react to generate phosphorus pentafluoride gas; and introducing the lithium fluoride solution and the phosphorus pentafluoride gas generated in the second microreactor into a third microreactor to react to obtain a lithium hexafluorophosphate synthetic liquid.
In one embodiment, chlorine and phosphorus trichloride are introduced into a first microreactor to react to synthesize phosphorus pentachloride gas; and introducing the hydrogen fluoride solution dissolved with the lithium fluoride and the phosphorus pentachloride gas synthesized in the first microreactor into a second microreactor to react to obtain a synthetic liquid of lithium hexafluorophosphate.
Preferably, the mol ratio of the chlorine to the phosphorus trichloride is 1:1.01-1.05, the reaction temperature of the chlorine and the phosphorus trichloride is controlled to be 150-170 ℃, and the reaction pressure is 0.1-1 MPa.
Preferably, the molar ratio of the phosphorus pentachloride gas to the anhydrous hydrogen fluoride is 1:1.01-1.15, the reaction temperature of the phosphorus pentachloride gas and the anhydrous hydrogen fluoride is controlled to be 20-100 ℃, and the reaction pressure is 0.1-1 MPa.
Preferably, the reaction temperature of the lithium fluoride and the phosphorus pentafluoride gas is controlled to be 0-20 ℃, and the reaction pressure is controlled to be 0.1-1 MPa.
The lithium hexafluorophosphate synthetic liquid is crystallized, filtered and dried to obtain the lithium hexafluorophosphate, and unreacted gas is recycled.
In order to achieve the above object, the present invention also provides an apparatus for preparing lithium hexafluorophosphate using a microreactor, comprising: the first microreactor is used for reacting chlorine with phosphorus trichloride to synthesize phosphorus pentachloride gas; and the second microreactor is used for reacting the phosphorus pentachloride gas.
In one embodiment, further comprising: and anhydrous hydrogen fluoride is introduced into the second microreactor to react with the phosphorus pentachloride gas to generate phosphorus pentafluoride gas, and a lithium fluoride solution is introduced into the third microreactor to react with the phosphorus pentafluoride gas to generate a lithium hexafluorophosphate synthetic solution.
In one embodiment, a hydrogen fluoride solution dissolved with lithium fluoride is introduced into the second microreactor to react with phosphorus pentachloride gas to generate a lithium hexafluorophosphate synthetic fluid.
Compared with the prior art, the invention has the following effects:
1. the invention adopts the microreactor to carry out chlorination and fluorination reactions, has high intermolecular heat transfer and mass transfer efficiency of reaction materials, improves the reaction efficiency, and can lead out reaction heat, thereby ensuring the safety.
2. The yield of the anhydrous hydrogen fluoride and the phosphorus pentafluoride is improved by 10-30%, so that the material consumption is reduced, the production cost can be reduced by 10-20%, the material consumption is reduced, the three wastes generated in the production process are further reduced, and the method is more environment-friendly.
3. The invention adopts the modular microreactor for reaction, can implement intelligent monitoring and control integration, can automatically control the whole processes of feeding, reaction and discharging, can automatically control parameters such as flow, temperature, pressure and the like in the reaction process, and is easier for intelligent and continuous production.
Drawings
FIG. 1 is a schematic view of an apparatus for producing lithium hexafluorophosphate using a microreactor in example 1 of the present invention;
FIG. 2 is a schematic view of an apparatus for producing lithium hexafluorophosphate using a microreactor in example 2 of the present invention;
FIG. 3 is a flow chart of a method for preparing lithium hexafluorophosphate by using a microreactor in example 3 of the present invention;
fig. 4 is a flowchart of a method for preparing lithium hexafluorophosphate by using a microreactor in example 6 of the present invention.
Detailed Description
The invention relates to the technical field of lithium hexafluorophosphate synthesis, and mainly aims to overcome the defects of low safety in the production process caused by violent chlorination and fluorination reactions and strong heat release in the reaction process in the prior art.
It should be noted that, in the description of the present invention, the moisture content of chlorine is less than 0.0001%, the purity of phosphorus trichloride is greater than 99.99%, the purity of anhydrous hydrogen fluoride is greater than 99.95%, and the purity of lithium fluoride is greater than 99.95%.
In the description of the present invention, it should be noted that the terms "first", "second", and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The present invention will be described in detail with reference to specific examples.
Example 1
In this embodiment, an apparatus for preparing lithium hexafluorophosphate by using a microreactor is provided, as shown in fig. 1, including: the device comprises a first microreactor 1, a second microreactor 2 and a third microreactor 3, wherein the first microreactor 1 is communicated with a flow meter 101 and a first metering pump 102, the flow meter 101 is used for metering the amount of chlorine introduced into the first microreactor 1, the first metering pump 102 is used for continuously introducing phosphorus trichloride liquid into the first microreactor 1 and metering the chlorine, and the first microreactor 1 is used for synthesizing phosphorus pentachloride by reacting chlorine with phosphorus trichloride. The first microreactor 1 is communicated with the second microreactor 2 to introduce the synthesized phosphorus pentachloride into the second microreactor 2.
The second microreactor 2 is communicated with a second metering pump 201, the second metering pump 201 is used for introducing anhydrous hydrogen fluoride into the second microreactor 2 and metering, and the second microreactor 2 is used for reacting phosphorus pentachloride with the anhydrous hydrogen fluoride to synthesize phosphorus pentafluoride gas.
In order to purify the generated phosphorus pentafluoride gas, the output end of the second microreactor 2 is communicated with a filter 202, and the filter 202 is communicated with the third microreactor 3 so that the filtered phosphorus pentafluoride gas is introduced into the third microreactor 3.
The third microreactor 3 is communicated with a third metering pump 301, the third metering pump 301 is used for introducing a lithium fluoride solution into the third microreactor 3, the third microreactor 3 is used for reacting the lithium fluoride solution with phosphorus pentafluoride gas to obtain a lithium hexafluorophosphate synthetic liquid, and the third microreactor 3 is a microchannel reactor. In order to ensure the phosphorus pentafluoride gas to react completely, a plurality of stages of third microreactors may be connected in series to allow the unreacted phosphorus pentafluoride gas to react sufficiently.
Since the lithium fluoride solution in this embodiment is formed by dissolving high-purity lithium fluoride in anhydrous hydrogen fluoride, the third microreactor 3 is also communicated with the dissolving tank 4, and the lithium fluoride solution in the dissolving tank 4 is introduced into the third microreactor 3 through the third metering pump 301.
In this embodiment, the third microreactor 3 is further communicated with a synthesis liquid tank 5, the lithium hexafluorophosphate synthesis liquid and unreacted gas obtained in the third microreactor 3 enter the synthesis liquid tank 5, the unreacted gas is recycled, the lithium hexafluorophosphate synthesis liquid enters the post-processing module 6 to be crystallized, filtered and dried to obtain a lithium hexafluorophosphate product, and the post-processing module 6 may be an integrated structure of crystallization, filtration and drying, or may be a separate structure.
The micro structure of the micro reactor in the micro reactor enables the micro reactor equipment to have a very large specific surface area which can be hundreds of times or even thousands of times of the specific surface area of the stirring kettle, so that the micro reactor has extremely good heat transfer and mass transfer capacity, can realize instant uniform mixing and efficient heat transfer of materials, and avoids the potential safety hazard problem caused by violent heat release.
It should be noted that the microreactor, the flow meter, the metering pump, the filter and the like used in the present invention are all existing products, and the detailed structure thereof will not be described again.
Example 2
In this embodiment, an apparatus for preparing lithium hexafluorophosphate by using a microreactor is provided, as shown in fig. 2, including: the device comprises a first microreactor 1 and a second microreactor 2, wherein the first microreactor 1 is communicated with a flow meter 101 and a first metering pump 102, the flow meter 101 is used for metering the amount of chlorine introduced into the first microreactor 1, the first metering pump 102 is used for continuously introducing phosphorus trichloride liquid into the first microreactor 1 and metering the chlorine, and the first microreactor 1 is used for synthesizing phosphorus pentachloride by reacting chlorine with phosphorus trichloride. The first microreactor 1 is communicated with the second microreactor 2 to introduce the synthesized phosphorus pentachloride into the second microreactor 2.
The second microreactor 2 is communicated with a second metering pump 201, the second metering pump 201 is used for introducing a lithium fluoride solution into the second microreactor 2 and metering, the second microreactor 2 is used for reacting phosphorus pentachloride, lithium fluoride and excessive hydrogen fluoride to synthesize a lithium hexafluorophosphate synthetic fluid, and the second microreactor is a microchannel reactor in the embodiment.
Since the lithium fluoride solution in this embodiment is formed by dissolving high-purity lithium fluoride into anhydrous hydrogen fluoride, the second microreactor 2 is also communicated with the dissolving tank 3, and the lithium fluoride solution in the dissolving tank 3 is introduced into the second microreactor 2 through the second metering pump 201.
In this embodiment, the second microreactor 2 is further communicated with a synthesis liquid tank 4, the lithium hexafluorophosphate synthesis liquid and the unreacted gas obtained in the second microreactor 2 enter the synthesis liquid tank 4, the unreacted gas is recycled, the lithium hexafluorophosphate synthesis liquid enters the post-processing module 5 to be crystallized, filtered and dried to obtain a lithium hexafluorophosphate product, and the post-processing module 5 may be an integral structure of crystallization, filtration and drying or a separate structure.
Example 3
This example provides a method for preparing lithium hexafluorophosphate by using a microreactor, which comprises using the apparatus of example 1, measuring chlorine gas by a flow meter 101, and controlling the introduction rate of chlorine gas to 70 g/min; starting the first metering pump 102, continuously introducing phosphorus trichloride into the first microreactor 1 to react with chlorine to generate phosphorus pentachloride, and controlling the introduction speed of the phosphorus trichloride to be 130g/min, wherein the molar ratio of chlorine to phosphorus trichloride is 1:1.01, the reaction temperature of chlorine and phosphorus trichloride is controlled to be 150 ℃, and the reaction pressure is 0.3 MPa.
The phosphorus pentachloride synthesized in the first microreactor 1 is led into a second microreactor 2, a second metering pump 201 is started, anhydrous hydrogen fluoride is continuously led into the second microreactor 2 to react with the phosphorus pentachloride to generate phosphorus pentafluoride gas, the leading-in speed of the anhydrous hydrogen fluoride is controlled to be 105g/min, the molar ratio of the phosphorus pentachloride to the anhydrous hydrogen fluoride is 1:1.05, the reaction temperature of the phosphorus pentachloride and the anhydrous hydrogen fluoride is controlled to be 80 ℃, and the reaction pressure is 0.3 MPa.
The generated phosphorus pentafluoride gas enters a filter 202 for filtration, and the filtered phosphorus pentafluoride gas enters the third microreactor 3. Preparing a lithium fluoride solution in a dissolving tank 4, specifically dissolving high-purity lithium fluoride in anhydrous hydrogen fluoride, starting a third metering pump 301 to continuously introduce the lithium fluoride solution in the dissolving tank 4 into a third microreactor 3 to react with phosphorus pentafluoride gas to generate a lithium hexafluorophosphate synthetic solution, controlling the introduction speed of the lithium fluoride solution to be 900g/min, controlling the reaction temperature of the lithium fluoride and the phosphorus pentafluoride to be 0 ℃, and controlling the reaction pressure to be 1 MPa.
And (3) introducing the lithium hexafluorophosphate synthetic liquid synthesized in the third microreactor 3 and unreacted gas into a synthetic liquid tank 5, wherein the concentration of lithium hexafluorophosphate in the synthetic liquid is 21%, the unreacted gas is recycled, the lithium hexafluorophosphate synthetic liquid enters a post-processing assembly 6 for processing, specifically, the lithium hexafluorophosphate synthetic liquid is crystallized, separated and dried in sequence to obtain a lithium hexafluorophosphate product, the yield of lithium hexafluorophosphate is 98%, and the purity of the product is 99.95%.
Example 4
Example 4 differs from example 3 in that: the mol ratio of the chlorine to the phosphorus trichloride is 1:1.05, the reaction temperature of the chlorine and the phosphorus trichloride is 170 ℃, and the reaction pressure is 0.1 MPa; the molar ratio of the phosphorus pentachloride to the anhydrous hydrogen fluoride is 1:1.15, the reaction temperature of the phosphorus pentachloride and the anhydrous hydrogen fluoride is 100 ℃, and the reaction pressure is 0.1 MPa; the reaction temperature of the lithium fluoride and the phosphorus pentafluoride is 20 ℃, and the reaction pressure is 0.1 MPa.
Example 5
Example 5 differs from example 3 in that: the mol ratio of chlorine to phosphorus trichloride is 1:1.03, the reaction temperature of the chlorine and the phosphorus trichloride is 160 ℃, and the reaction pressure is 1 MPa; the molar ratio of the phosphorus pentachloride to the anhydrous hydrogen fluoride is 1:1.01, the reaction temperature of the phosphorus pentachloride and the anhydrous hydrogen fluoride is 20 ℃, and the reaction pressure is 1 MPa; the reaction temperature of the lithium fluoride and the phosphorus pentafluoride is 0 ℃, and the reaction pressure is 1 MPa.
Example 6
This example provides a method for preparing lithium hexafluorophosphate by using a microreactor, which comprises using the apparatus of example 2, measuring chlorine gas by a flow meter 101, and controlling the introduction rate of chlorine gas to 70 g/min; starting the first metering pump 102, continuously introducing phosphorus trichloride into the first microreactor 1, wherein the introduction speed of the phosphorus trichloride is controlled to be 130g/min, the molar ratio of chlorine to phosphorus trichloride is 1:1.01, the reaction temperature of the chlorine and the phosphorus trichloride is controlled to be 150 ℃, and the reaction pressure is 0.3 MPa.
The phosphorus pentachloride synthesized in the first microreactor 1 is introduced into a second microreactor 2, a lithium fluoride solution is prepared in a dissolving tank 4, specifically, high-purity lithium fluoride is dissolved in anhydrous hydrogen fluoride, then a second metering pump 201 is started, the lithium fluoride solution in the dissolving tank 4 is continuously introduced into the second microreactor 2 to react with the phosphorus pentachloride to generate a lithium hexafluorophosphate synthetic solution, the introduction speed of the lithium fluoride solution is controlled to be 1000g/min, the reaction temperature of the phosphorus pentachloride and the lithium fluoride is 10-15 ℃, and the reaction pressure is 0.3 MPa.
And (3) introducing the lithium hexafluorophosphate synthetic liquid synthesized in the second microreactor 2 and unreacted gas into a synthetic liquid tank 4, wherein the concentration of lithium hexafluorophosphate in the synthetic liquid is 20%, the unreacted gas is recycled, the lithium hexafluorophosphate synthetic liquid enters a post-treatment assembly 5 for treatment, specifically, the lithium hexafluorophosphate synthetic liquid is crystallized, separated and dried in sequence to obtain a lithium hexafluorophosphate product, the yield of lithium hexafluorophosphate is 97%, and the purity of the product is 99.95%.
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. A method for preparing lithium hexafluorophosphate by using a microreactor is characterized in that chlorine, phosphorus trichloride, anhydrous hydrogen fluoride and a lithium fluoride solution are introduced into the microreactor to react so as to realize instant uniform mixing and rapid reaction of materials and to guide out reaction heat.
2. The method for preparing lithium hexafluorophosphate by using the microreactor as claimed in claim 1, wherein chlorine and phosphorus trichloride are introduced into the first microreactor to react to synthesize phosphorus pentachloride gas;
introducing anhydrous hydrogen fluoride and phosphorus pentachloride gas synthesized in the first microreactor into a second microreactor to react to generate phosphorus pentafluoride gas;
and introducing the lithium fluoride solution and the phosphorus pentafluoride gas generated in the second microreactor into a third microreactor to react to obtain a lithium hexafluorophosphate synthetic liquid.
3. The method for preparing lithium hexafluorophosphate by using the microreactor as claimed in claim 1, wherein chlorine and phosphorus trichloride are introduced into the first microreactor to react to synthesize phosphorus pentachloride gas;
and introducing the hydrogen fluoride solution dissolved with the lithium fluoride and the phosphorus pentachloride gas synthesized in the first microreactor into a second microreactor to react to obtain a synthetic liquid of lithium hexafluorophosphate.
4. The method for preparing lithium hexafluorophosphate by using the microreactor as claimed in claim 2 or 3, wherein the molar ratio of chlorine gas to phosphorus trichloride is 1:1.01-1.05, the reaction temperature of chlorine gas and phosphorus trichloride is controlled at 150-170 ℃, and the reaction pressure is controlled at 0.1-1 MPa.
5. The method for preparing lithium hexafluorophosphate by using the microreactor as claimed in claim 2, wherein the molar ratio of phosphorus pentachloride gas to anhydrous hydrogen fluoride is 1:1.01-1.15, the reaction temperature of phosphorus pentachloride gas and hydrogen fluoride is controlled to be 20-100 ℃, and the reaction pressure is controlled to be 0.1-1 MPa.
6. The method for producing lithium hexafluorophosphate using a microreactor according to claim 2, wherein the reaction temperature of lithium fluoride with the phosphorus pentafluoride gas is controlled to 0 to 20 ℃ and the reaction pressure is controlled to 0.1 to 1 MPa.
7. The method for preparing lithium hexafluorophosphate by using the microreactor according to claim 2 or 3, wherein lithium hexafluorophosphate is obtained by crystallizing, filtering and drying the lithium hexafluorophosphate synthetic liquid, and gases which are not completely reacted are recycled.
8. An apparatus for preparing lithium hexafluorophosphate by using a microreactor, comprising:
the first microreactor is used for reacting chlorine with phosphorus trichloride to synthesize phosphorus pentachloride gas;
and the second microreactor is used for reacting the phosphorus pentachloride gas.
9. The apparatus for preparing lithium hexafluorophosphate using a microreactor according to claim 8, further comprising: and anhydrous hydrogen fluoride is introduced into the second microreactor to react with the phosphorus pentachloride gas to generate phosphorus pentafluoride gas, and a lithium fluoride solution is introduced into the third microreactor to react with the phosphorus pentafluoride gas to generate a lithium hexafluorophosphate synthetic solution.
10. The apparatus of claim 8, wherein the second microreactor is adapted to introduce a solution of hydrogen fluoride with dissolved lithium fluoride into the second microreactor for reaction with phosphorus pentachloride gas to form a lithium hexafluorophosphate synthesis solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919504A (en) * | 2021-03-18 | 2021-06-08 | 湖北迈可凯科技有限公司 | Method and device for synthesizing lithium hexafluorophosphate by adopting continuous flow reactor |
| CN113104825A (en) * | 2021-04-01 | 2021-07-13 | 多氟多化工股份有限公司 | Preparation method of phosphorus chloride |
| CN115586755A (en) * | 2022-10-28 | 2023-01-10 | 福建省龙德新能源有限公司 | Production management control system and method for preparing lithium hexafluorophosphate |
-
2019
- 2019-12-30 CN CN201911394711.0A patent/CN110937587A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919504A (en) * | 2021-03-18 | 2021-06-08 | 湖北迈可凯科技有限公司 | Method and device for synthesizing lithium hexafluorophosphate by adopting continuous flow reactor |
| CN112919504B (en) * | 2021-03-18 | 2023-02-17 | 湖北迈可凯科技有限公司 | Method and device for synthesizing lithium hexafluorophosphate by adopting continuous flow reactor |
| CN113104825A (en) * | 2021-04-01 | 2021-07-13 | 多氟多化工股份有限公司 | Preparation method of phosphorus chloride |
| CN115586755A (en) * | 2022-10-28 | 2023-01-10 | 福建省龙德新能源有限公司 | Production management control system and method for preparing lithium hexafluorophosphate |
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