CN211078479U - Lithium hexafluorophosphate reactor - Google Patents

Lithium hexafluorophosphate reactor Download PDF

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Publication number
CN211078479U
CN211078479U CN201922292710.7U CN201922292710U CN211078479U CN 211078479 U CN211078479 U CN 211078479U CN 201922292710 U CN201922292710 U CN 201922292710U CN 211078479 U CN211078479 U CN 211078479U
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China
Prior art keywords
reactor
pipe
phosphorus pentafluoride
lithium hexafluorophosphate
valve
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CN201922292710.7U
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Inventor
杨瑞甫
肖文绪
肖丰贤
周利彬
陈东林
吴远胜
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Fujian Longde new energy Co.,Ltd.
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Fujian Longde New Energy Co ltd
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Abstract

The utility model provides a lithium hexafluorophosphate reactor, advance pipe, lithium hexafluorophosphate mother liquor export and agitator including reactor body, phosphorus pentafluoride gas, the stirring end of agitator stretches into this is internal to the reactor, the stiff end of agitator is fixed on the lateral wall of reactor body, its characterized in that: the cleaning system is used for cleaning the phosphorus pentafluoride gas inlet pipe; the phosphorus pentafluoride gas inlet pipe is parallel to the shaft of the stirrer and is connected with the stirrer, so that the reaction efficiency is high, and the pipeline is prevented from being blocked by crystallization.

Description

Lithium hexafluorophosphate reactor
Technical Field
The utility model relates to a lithium hexafluorophosphate reactor belongs to lithium hexafluorophosphate preparation technical field.
Background
Lithium hexafluorophosphate is a main raw material of lithium ion battery electrolyte, and is the most commonly used electrolyte lithium salt at present because of good ionic conductivity and electrochemical stability, the lithium hexafluorophosphate synthesis method has the advantages of a gas-solid method, a solvent method, an ion exchange method and the like, and a hydrogen fluoride solvent method which uses anhydrous hydrogen fluoride as a solvent and lithium fluoride as a solute and introduces phosphorus pentafluoride gas for synthesis has the advantages of high product purity, moderate cost and the like, and is the main method for realizing industrialized production at present, as shown in fig. 1, the hydrogen fluoride solvent method is a method for dissolving lithium fluoride in anhydrous hydrogen fluoride in a reactor body 01 to form L iF solution of HF, introducing high-purity phosphorus pentafluoride gas from a phosphorus pentafluoride gas inlet pipe 02 for reaction, and the obtained lithium hexafluorophosphate product mother liquor is discharged from a lithium hexafluorophosphate product outlet 03, the reaction has the following defects that (1) the synthesis reaction utilizes L iF in gas-phase phosphorus pentafluoride and anhydrous hydrogen fluoride for reaction, the reaction belongs to a multiphase reaction, the reaction efficiency is influenced by gas-phase interface, liquid-phase reaction rate and gas-liquid-phase reaction rate, thus the reaction rate, the reaction rate is influenced by the gas-phase phosphorus pentafluoride gas-phase condensation reaction, the gas-phase reaction, the reaction efficiency is reduced, and the lithium hexafluorophosphate product is reduced, the lithium fluoride-phase reaction efficiency is reduced, and the lithium-phase reaction efficiency is reduced, the lithium fluoride-phase reaction efficiency is reduced.
SUMMERY OF THE UTILITY MODEL
The utility model provides a, can effectively solve above-mentioned problem.
The utility model discloses a realize like this:
a lithium hexafluorophosphate reactor comprises a reactor body, a phosphorus pentafluoride gas inlet pipe, a lithium hexafluorophosphate mother liquor outlet and a stirrer, wherein the stirring end of the stirrer extends into the reactor body, and the fixed end of the stirrer is fixed on the side wall of the reactor body; the cleaning system is used for cleaning the phosphorus pentafluoride gas inlet pipe; the phosphorus pentafluoride gas inlet pipe is parallel to the shaft of the stirrer and connected with the stirrer, and the outlet of the phosphorus pentafluoride gas inlet pipe is close to the stirring paddle of the stirrer.
As further modified, cleaning system is including encircleing the ring pipe of reactor body periphery, be equipped with outer air inlet on the ring pipe, the gaseous pipe UNICOM that advances of phosphorus pentafluoride the ring pipe, on the ring pipe outer air inlet with the gaseous pipe of advancing of phosphorus pentafluoride sets up first valve between the pipe, still be equipped with the scavenge pipe on the ring pipe and let in the reactor is originally internal, set up the second valve on the scavenge pipe, on the ring pipe the scavenge pipe with the gaseous pipe of advancing of phosphorus pentafluoride sets up the third valve between the pipe.
As a further improvement, the outside wall of the reactor body is provided with a replacement heat jacket.
As a further improvement, the number of the stirrers is at least 2.
As a further improvement, the reactor body, the stirrer and the phosphorus pentafluoride gas inlet pipe are made of corrosion-resistant materials.
As a further improvement, a liquid level meter, a thermometer and a pressure gauge are also arranged on the reactor body.
As a further improvement, the reactor body is also provided with an exhaust gas discharge port.
As a further improvement, a check valve is arranged on the outer air inlet.
As a further improvement, the first valve, the second valve and the third valve are automatic valves or manual valves.
As a further improvement, the phosphorus pentafluoride gas inlet pipe is positioned in the shaft of the stirrer.
The utility model has the advantages that:
the utility model discloses an among the lithium hexafluorophosphate reactor, the gaseous pipe that advances of phosphorus pentafluoride with the axle of agitator is parallel and even together, the gaseous export of advancing the pipe of phosphorus pentafluoride is close to the stirring rake of agitator, follows when phosphorus pentafluoride gas advances the pipe and lets in the reactor is internal, and phosphorus pentafluoride is gaseous once gets into this internal, just is stirred by the agitator, rapidly with L iF HF solution misce bene, and reaction efficiency is high.
The utility model discloses a lithium hexafluorophosphate reactor has set up the cleaning system who is used for wasing phosphorus pentafluoride gas and advances the pipe, and when being in the reaction stage that admits air, second valve and third valve are in the closed condition, and phosphorus pentafluoride gas advances the pipe by phosphorus pentafluoride gas and gets into the reactor body in, reacts; after cleaning system starts, first valve is closed, and corresponding second valve and third valve are opened, and this internal solution of reactor is followed the scavenge pipe gets into in the ring pipe, by gaseous admission pipe of phosphorus pentafluoride gets back to this is internal to the reactor, it is right simultaneously gaseous admission pipe of phosphorus pentafluoride washes, washes and accomplishes back second valve, third valve and close, and first valve is opened and is continued to admit air and react, and it is further gaseous to advance the pipe to carry out regularly clearance to the phosphorus pentafluoride of this cleaning system to see that this cleaning system is further, and the effectual unobstructed of phosphorus pentafluoride gas admission pipe of having guaranteed reduces the cost and the safety risk of operation.
The utility model discloses a quantity of lithium hexafluorophosphate reactor's agitator is 2 sets at least, and a plurality of agitators make solution intensive mixing, reduce the blind spot that does not circulate, have improved the area of contact of phosphorus pentafluoride gas and L iF solution gas-liquid reaction greatly, reduce the composition of L iF impurity in the product, have improved phosphorus pentafluoride's utilization ratio, have improved product purity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Figure 1 is a schematic diagram of a prior art lithium hexafluorophosphate reactor configuration.
Fig. 2 is a schematic structural diagram of a lithium hexafluorophosphate reactor of the present invention.
Figure 3 is the piping diagram of the cleaning system of the lithium hexafluorophosphate reactor of the present invention.
Reference numerals: the reactor comprises a reactor body 1, a phosphorus pentafluoride gas inlet pipe 2, a lithium hexafluorophosphate mother liquor outlet 3, a stirrer 4, a ring pipe 5, an external gas inlet 6, a first valve 7, a cleaning pipe 8, a second valve 9, a third valve 10, a heat exchange jacket 11 and a check valve 12.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the drawings of the embodiments of the present invention are combined to clearly and completely describe the technical solutions of the embodiments of the present invention, and obviously, the described embodiments are some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the accompanying drawings, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise.
Referring to fig. 2 to 3, the utility model provides a lithium hexafluorophosphate reactor, including reactor body 1, phosphorus pentafluoride gas advance pipe 2, lithium hexafluorophosphate mother liquor export 3 and agitator 4, the stirring end of agitator 4 stretches into in the reactor body 1, the stiff end of agitator 4 is fixed on the lateral wall of reactor body 1, still include the cleaning system who is used for wasing phosphorus pentafluoride gas and advances pipe 2, phosphorus pentafluoride gas advances pipe 2 and links together with the axle of agitator 4 is parallel, the export that phosphorus pentafluoride gas advances pipe 2 is close to the stirring rake of agitator 4. when phosphorus pentafluoride gas advances pipe 2 from the phosphorus pentafluoride gas and lets in the reactor body 1, phosphorus pentafluoride gas is once got into reactor body 1, just is stirred by agitator 4, mixes with L iF HF solution rapidly, and the reaction efficiency is high in addition, the lithium hexafluorophosphate that produces is thrown away by agitator 4's centrifugal force rapidly, can prevent that it from phosphorus pentafluoride gas advances pipe 2, the pipeline that need not dredged the transportation safety and carried out the reduction of the cost of frequently transporting with the shutoff.
Cleaning system is including encircleing in the ring pipe 5 of 1 periphery of reactor body, be equipped with outer air inlet 6 on the ring pipe 5, phosphorus pentafluoride gas advances pipe 2 UNICOM the ring pipe 5, be in on the ring pipe 5 outer air inlet 6 with phosphorus pentafluoride gas advances and sets up first valve 7 between the pipe 2, still be equipped with scavenge pipe 8 on the ring pipe 5 and let in the reactor body 1, set up second valve 9 on the scavenge pipe 8, be in on the ring pipe scavenge pipe 8 with phosphorus pentafluoride gas advances and sets up third valve 10 between the pipe 2. The reaction of the feed gas and the purging may be performed alternately. When the reactor is in the gas inlet reaction stage, the second valve 9 and the third valve 10 are in the closed state, the first valve 7 is opened, phosphorus pentafluoride gas enters the annular pipe 5 from the outer gas inlet pipe 6, and then enters the reactor body 1 from the phosphorus pentafluoride gas inlet pipe 2 to react. After cleaning system starts, first valve 7 closes, and corresponding second valve 9 and third valve 10 are opened, and solution in the reactor body 1 is followed the scavenge pipe 8 gets into in the ring pipe 1, by gaseous pipe 2 that advances of phosphorus pentafluoride gets back to in the reactor body 1, it is right simultaneously gaseous pipe 2 that advances of phosphorus pentafluoride washes, and wash and accomplish back second valve 9, third valve 10 and close, and first valve 7 is opened and is continued to admit air and react, and it is further that this cleaning system advances pipe 2 to the phosphorus pentafluoride and regularly clear up, the effectual unobstructed gaseous pipe that advances of phosphorus pentafluoride of having guaranteed, reduces the cost and the safety risk of operation.
The wall of the reactor body 1 is externally provided with a replacement heat jacket 11, and the temperature of the reactor is reduced by a coolant of 20 ℃, so that the reaction is carried out at a low temperature, and the hydrogen fluoride is prevented from being volatilized and wasted.
The quantity of agitator 4 is 2 sets at least, a plurality of agitators 4 make the solution intensive mixing, reduce the blind spot that does not circulate, improved the area of contact of phosphorus pentafluoride gas with L iF solution gas-liquid reaction greatly, reduce the composition of L iF impurity in the product, improved the utilization ratio of phosphorus pentafluoride, improved product purity.
Lithium hexafluorophosphate mother liquor export 3 sets up the bottom of reactor body 1 makes things convenient for the product to discharge.
The reactor body 1 is also provided with a liquid level meter, a thermometer and a pressure gauge, so that the reaction condition can be monitored in real time.
The reactor body 1 is also provided with an exhaust gas discharge port.
The outer air inlet is provided with a check valve 12 to prevent the medium from back streaming.
The first valve 7, the second valve 9 and the third valve 10 are automatic valves or manual valves. When the valve is an automatic valve, the valve can be automatically controlled by connecting a controller.
Gaseous admission pipe 2 of phosphorus pentafluoride is located in the axle of agitator 4 not only practices thrift reaction space, and phosphorus pentafluoride is gaseous just getting into by agitator 4 stirring once moreover, and reaction efficiency is high, prevents that the crystallization from blockking up the pipeline.
The reactor body 1, the stirrer 4 and the phosphorus pentafluoride gas inlet pipe are made of corrosion-resistant materials, including but not limited to 316L, hastelloy, monel, dual-phase steel and the like.
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 protection scope of the present invention.

Claims (10)

1. The utility model provides a lithium hexafluorophosphate reactor, advances pipe, lithium hexafluorophosphate mother liquor export and agitator including reactor body, phosphorus pentafluoride gas, the stirring end of agitator stretches into this is internal to the reactor, the stiff end of agitator is fixed on the lateral wall of reactor body, its characterized in that: the cleaning system is used for cleaning the phosphorus pentafluoride gas inlet pipe; the phosphorus pentafluoride gas inlet pipe is parallel to the shaft of the stirrer and connected with the stirrer, and the outlet of the phosphorus pentafluoride gas inlet pipe is close to the stirring paddle of the stirrer.
2. The lithium hexafluorophosphate reactor of claim 1, wherein: cleaning system is including encircleing the ring pipe of reactor body periphery, be equipped with outer air inlet on the ring pipe, phosphorus pentafluoride gas advances a tub UNICOM the ring pipe, on the ring pipe outer air inlet with phosphorus pentafluoride gas advances to set up first valve between the pipe, still be equipped with the scavenge pipe on the ring pipe and let in the reactor is originally internal, set up the second valve on the scavenge pipe, on the ring pipe the scavenge pipe with phosphorus pentafluoride gas advances to set up the third valve between the pipe.
3. The lithium hexafluorophosphate reactor of claim 1, wherein: a replacement heat jacket is arranged outside the wall of the reactor body.
4. The lithium hexafluorophosphate reactor of claim 1, wherein: the number of the stirrers is at least 2.
5. The lithium hexafluorophosphate reactor of claim 1, wherein: the reactor body, the stirrer and the phosphorus pentafluoride gas inlet pipe are made of corrosion-resistant materials.
6. The lithium hexafluorophosphate reactor of claim 1, wherein: the reactor body is also provided with a liquid level meter, a thermometer and a pressure gauge.
7. The lithium hexafluorophosphate reactor of claim 1, wherein: the reactor body is also provided with an exhaust gas discharge port.
8. The lithium hexafluorophosphate reactor of claim 2, wherein: and a check valve is arranged on the outer air inlet.
9. The lithium hexafluorophosphate reactor of claim 2, wherein: the first valve, the second valve and the third valve are automatic valves or manual valves.
10. The lithium hexafluorophosphate reactor of claim 2, wherein: the phosphorus pentafluoride gas inlet pipe is positioned in the shaft of the stirrer.
CN201922292710.7U 2019-12-19 2019-12-19 Lithium hexafluorophosphate reactor Active CN211078479U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113772695A (en) * 2021-10-21 2021-12-10 福建省龙德新能源有限公司 High-efficiency synthesis method of lithium hexafluorophosphate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113772695A (en) * 2021-10-21 2021-12-10 福建省龙德新能源有限公司 High-efficiency synthesis method of lithium hexafluorophosphate

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Address after: No. 30, Gongye Road, Pingpu village, Jiaoyang Town, Shanghang County, Longyan City, Fujian Province, 364000

Patentee after: Fujian Longde new energy Co.,Ltd.

Address before: 364000 Jiaoyang Industrial Development Zone, Shanghang County, Longyan City, Fujian Province

Patentee before: Fujian Longde new energy Co.,Ltd.

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