A lithium hexafluorophosphate synthesis reaction device

Abstract

This utility model relates to a lithium hexafluorophosphate synthesis reaction apparatus. The technical solution is as follows: a jacket is provided on the outside of the reactor; a first refrigerant inlet valve is provided at the bottom of the jacket; a second refrigerant outlet valve is provided at the top of the jacket; a liquid phase outlet is provided at the center of the lower part of the reactor; baffles are welded to the inner wall of the reactor; and a lithium fluoride hydrogen fluoride mother liquor inlet, a tail gas outlet, a stirring paddle, and a phosphorus pentafluoride gas phase inlet are provided at the top of the reactor. The phosphorus pentafluoride gas phase inlet is connected to a gas distributor through the reactor's inlet pipe. The beneficial effects are: the gas distributor allows for more dispersed gas entry into the reactor, improving the dispersion of the reactant gas in the reaction liquid, increasing the reaction rate and the utilization rate of the reaction liquid; the baffles enhance the mixing effect between the mixed reaction liquid and the reactant gas, thereby increasing the reaction rate; and the tail gas is discharged after partially removing hydrogen fluoride through a demister.

Description

Technical Field

[0001] This utility model relates to the field of lithium hexafluorophosphate preparation technology, and in particular to a lithium hexafluorophosphate synthesis reaction apparatus. Background Technology

[0002] Currently, the mainstream preparation process for lithium hexafluorophosphate (LiPF6) both domestically and internationally is the hydrofluoric acid solvent method. This process involves dissolving lithium fluoride in anhydrous hydrogen fluoride to prepare a lithium fluoride hydrogen fluoride solution, then introducing phosphorus pentafluoride gas into the solution to initiate a gas-liquid reaction and generate a lithium hexafluorophosphate synthesis liquid. The product is then obtained through crystallization and drying. However, existing synthesis reactors often suffer from several problems: Firstly, existing reactors typically introduce phosphorus pentafluoride gas directly into the reaction liquid via a single insertion tube, resulting in low reaction rates and low phosphorus pentafluoride utilization. Secondly, the stirring in existing reactors only involves unidirectional rotation, leading to insufficient mixing of the reaction liquid and phosphorus pentafluoride gas, further contributing to the low reaction rate. Utility Model Content

[0003] The purpose of this invention is to address the aforementioned deficiencies in the existing technology by providing a lithium hexafluorophosphate synthesis reaction apparatus that not only improves the utilization rate of phosphorus pentafluoride gas but also increases the reaction rate.

[0004] The present invention relates to a lithium hexafluorophosphate synthesis reaction apparatus, the technical solution of which includes a jacket (1), a baffle (2), a hydrogen fluoride mother liquor inlet (3), a tail gas outlet (4), a stirring paddle (5), a phosphorus pentafluoride gas phase inlet (6), a first refrigerant inlet valve (7), a second refrigerant outlet valve (8), a discharge port (9), a reaction vessel (10), and a gas distributor (11). The reaction vessel (10) is provided with a jacket (1) on its outer side. The bottom of the jacket (1) is provided with a first refrigerant inlet valve (7), and the top of the jacket (1) is provided with a... There is a second refrigerant outlet valve (8), and a liquid phase outlet (9) is provided at the center of the lower part of the reactor (10). A baffle (2) is welded on the inner wall of the reactor (10). The top of the reactor (10) is provided with a lithium fluoride hydrogen fluoride mother liquor inlet (3), a tail gas outlet (4), a stirring paddle (5) and a phosphorus pentafluoride gas phase inlet (6). The phosphorus pentafluoride gas phase inlet (6) is connected to the gas inlet pipe (13) of the reactor (10). The lower end of the gas inlet pipe (13) is connected to the gas distributor (11) placed on the lower part of the inner wall of the reactor (10).

[0005] Preferably, the above-mentioned stirring paddle (5) is provided with three sets of coaxial stirring blades, which are respectively arranged in the lower part, middle part and upper middle part of the liquid phase.

[0006] Preferably, the baffle (2) is disposed on the inner wall of the reactor (10) and is set at 60° to the outer tangent of the inner wall of the reactor (10).

[0007] Preferably, the lower end of the above-mentioned air inlet pipe (13) is connected to a gas distributor (11) for gas distribution. The gas distributor (11) adopts a ring structure or a circular structure, and air outlet holes are evenly opened in the lower part of the pipe wall.

[0008] Preferably, the aforementioned stirring paddle (5) is connected to the top cover of the reactor (10) via a bearing with a magnetohydrodynamic seal.

[0009] Preferably, the exhaust port (4) is externally connected to a demister (14).

[0010] Preferably, the top of the above-mentioned reaction vessel (10) is provided with a radar level gauge port (12).

[0011] The beneficial effects of this invention are as follows: By adding lithium fluoride mother liquor into the reactor through the feed inlet, phosphorus pentafluoride gas can be more dispersed into the reactor body through the gas distributor, improving the dispersion of the reaction gas in the reaction liquid, and increasing the reaction rate and utilization rate of the reaction liquid; the stirring paddle makes the solution in the reactor in a downward and upward pressure state, and the baffle plate enhances the mixing effect of the mixed reaction liquid and the reaction gas, thereby improving the reaction rate; after the reaction, the tail gas is discharged after partially intercepting hydrogen fluoride through the demister. Attached Figure Description

[0012] Figure 1 This is a schematic diagram of the structure of this utility model; Figure 2 This is a schematic diagram of the installation of the reactor baffle. Figure 3 This is a partially enlarged schematic diagram of the installation of the reactor baffle; In the diagram above: 1. Jacket; 2. Baffle; 3. Hydrogen fluoride mother liquor inlet; 4. Tail gas outlet; 5. Stirring paddle; 6. Phosphorus pentafluoride gas phase inlet; 7. First refrigerant inlet valve; 8. Second refrigerant outlet valve; 9. Discharge outlet; 10. Reactor; 11. Gas distributor; 12. Radar level gauge port; 13. Inlet pipe; 14. Demister. Detailed Implementation

[0013] The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0014] Example 1, referring to Figures 1-3The present invention relates to a lithium hexafluorophosphate synthesis reaction apparatus, comprising a jacket 1, a baffle 2, a hydrogen fluoride mother liquor inlet 3, a tail gas outlet 4, a stirring paddle 5, a phosphorus pentafluoride gas phase inlet 6, a first refrigerant inlet valve 7, a second refrigerant outlet valve 8, a discharge outlet 9, a reactor 10, and a gas distributor 11. The reactor 10 is provided with a jacket 1 on its outer side, a first refrigerant inlet valve 7 at the bottom of the jacket 1, a second refrigerant outlet valve 8 at the top of the jacket 1, a liquid phase discharge outlet 9 at the center of the lower part of the reactor 10, a baffle 2 welded to the inner wall of the reactor 10, and a lithium fluoride hydrogen fluoride mother liquor inlet 3, a tail gas outlet 4, a stirring paddle 5, and a phosphorus pentafluoride gas phase inlet 6 at the top of the reactor 10. The phosphorus pentafluoride gas phase inlet 6 is connected to the gas inlet pipe 13 of the reactor 10, and the lower end of the gas inlet pipe 13 is connected to the gas distributor 11 placed on the lower part of the inner wall of the reactor 10.

[0015] The aforementioned stirring paddle 5 is equipped with three sets of coaxial stirring blades, which are respectively arranged in the lower, middle and upper middle parts of the liquid phase.

[0016] The aforementioned baffle 2 is installed on the inner wall of the reactor 10, and is set at 60° to the outer tangent of the inner wall of the reactor 10, and is arranged in a ring to prevent the liquid from generating vortices and enhance the mixing effect.

[0017] The lower end of the aforementioned air inlet pipe 13 is connected to a gas distributor 11 for gas distribution. The gas distributor 11 has a circular structure and air outlet holes are evenly opened in the lower part of the pipe wall.

[0018] The aforementioned stirring paddle 5 is connected to the top cover of the reactor 10 via a bearing with a magnetohydrodynamic seal.

[0019] The exhaust port 4 mentioned above is externally connected to a demister 14.

[0020] The reactor 10 described above is equipped with a radar level gauge port 12 at its top.

[0021] In use, lithium fluoride mother liquor is added into the reactor 10 through the feed inlet 3, and phosphorus pentafluoride gas is added into the reactor 10 through the phosphorus pentafluoride gas inlet 6. The phosphorus pentafluoride gas can be more dispersed into the reactor through the gas distributor 11, which improves the dispersion of the reaction gas in the reaction liquid, and increases the reaction rate and the utilization rate of the reaction liquid. The stirring paddle 5 is started, and the solution in the reactor is in a downward and upward pressure state by the stirring paddle. At the same time, the baffle 2 with a 60-degree angle to the outer tangent can prevent the liquid from generating vortices, enhance the mixing effect of the mixed reaction liquid and the reaction gas, and thus improve the reaction rate. The cooling medium is introduced into the jacket 1 to cool the liquid. The reacted liquid is discharged through the discharge port 9 at the bottom, and the tail gas is discharged after the demister 14 intercepts part of the hydrogen fluoride.

[0022] Example 2: A lithium hexafluorophosphate synthesis reactor mentioned in this utility model includes a jacket 1, a baffle 2, a hydrogen fluoride mother liquor inlet 3, a tail gas outlet 4, a stirring paddle 5, a phosphorus pentafluoride gas phase inlet 6, a first refrigerant inlet valve 7, a second refrigerant outlet valve 8, a discharge outlet 9, a reactor 10, and a gas distributor 11. The reactor 10 is equipped with a jacket 1 on its outer side. The bottom of the jacket 1 is equipped with the first refrigerant inlet valve 7, and the top of the jacket 1 is equipped with... The second refrigerant outlet valve 8 has a liquid phase outlet 9 located at the center of the lower part of the reactor 10. The inner wall of the reactor 10 is welded with a baffle 2. The top of the reactor 10 is equipped with a lithium fluoride hydrogen fluoride mother liquor inlet 3, a tail gas outlet 4, a stirring paddle 5, and a phosphorus pentafluoride gas phase inlet 6. The phosphorus pentafluoride gas phase inlet 6 is connected to the gas inlet pipe 13 of the reactor 10. The lower end of the gas inlet pipe 13 is connected to the gas distributor 11 placed on the lower part of the inner wall of the reactor 10.

[0023] The difference from Example 1 is: The lower end of the air inlet pipe 13 mentioned in this embodiment is connected to the gas distributor 11 for gas distribution. The gas distributor 11 adopts a circular structure and has air outlet holes of different sizes on the pipe wall, which can better disperse the raw material gas.

[0024] The above description is merely a preferred embodiment of this utility model. Any person skilled in the art may modify this utility model or modify it into an equivalent technical solution using the technical solutions described above. Therefore, any simple modifications or equivalent transformations made based on the technical solutions of this utility model are within the scope of protection claimed by this utility model.

Claims

1. A lithium hexafluorophosphate synthesis reaction apparatus, characterized in that: The reactor includes a jacket (1), a baffle (2), a hydrogen fluoride mother liquor inlet (3), a tail gas outlet (4), a stirring paddle (5), a phosphorus pentafluoride gas phase inlet (6), a first refrigerant inlet valve (7), a second refrigerant outlet valve (8), a discharge port (9), a reactor (10), and a gas distributor (11). The reactor (10) is equipped with a jacket (1) on its outer side. The bottom of the jacket (1) is equipped with a first refrigerant inlet valve (7), and the top of the jacket (1) is equipped with a second refrigerant outlet valve (8). The reactor (10) has a liquid outlet (9) at the center of its lower part. The reactor (10) has a baffle (2) welded to its inner wall. The reactor (10) has a lithium fluoride hydrogen fluoride mother liquor inlet (3), a tail gas outlet (4), a stirring paddle (5), and a phosphorus pentafluoride gas phase inlet (6) at its top. The phosphorus pentafluoride gas phase inlet (6) is connected to the gas inlet pipe (13) of the reactor (10). The lower end of the gas inlet pipe (13) is connected to the gas distributor (11) placed on the lower part of the inner wall of the reactor (10).

2. The lithium hexafluorophosphate synthesis reaction apparatus according to claim 1, characterized in that: The stirring paddle (5) is equipped with three sets of coaxial stirring blades, which are respectively arranged in the lower, middle and upper middle parts of the liquid phase.

3. The lithium hexafluorophosphate synthesis reaction apparatus according to claim 2, characterized in that: The baffle (2) is set on the inner wall of the reactor (10) and is set at 60° to the outer tangent of the inner wall of the reactor (10).

4. The lithium hexafluorophosphate synthesis reaction apparatus according to claim 3, characterized in that: The lower end of the air inlet pipe (13) is connected to a gas distributor (11) for gas distribution. The gas distributor (11) adopts a ring-shaped or circular structure and has uniformly opened air outlet holes in the lower part of the pipe wall.

5. The lithium hexafluorophosphate synthesis reaction apparatus according to claim 2, characterized in that: The stirring paddle (5) is connected to the top cover of the reactor (10) via a bearing with a magnetohydrodynamic seal.

6. The lithium hexafluorophosphate synthesis reaction apparatus according to claim 1, characterized in that: The exhaust port (4) is externally connected to a demister (14).

7. The lithium hexafluorophosphate synthesis reaction apparatus according to claim 1, characterized in that: The top of the reactor (10) is equipped with a radar level gauge port (12).

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