An apparatus for synthesizing lithium sulfide

Abstract

The utility model relates to lithium battery preparation technical field especially relates to a device of synthetic lithium sulfide, including integrated reation kettle, the top of reation kettle is fixedly connected with one end of exhaust pipe, the bottom in reation kettle is equipped with heating mechanism, be equipped with stirring mechanism in reation kettle, the middle part inner wall of reation kettle is fixedly equipped with the baffle of inclined setting, the baffle is annular, the outer peripheral wall of baffle with reation kettle's inner wall fixed connection, the baffle is gradually inclined setting from outside to its inside to downward; The bottom of reation kettle is equipped with air inlet, the air inlet passes through the pipeline and is connected with outside hydrogen sulfide gas source, the upper portion of reation kettle is equipped with feed inlet, the bottom of reation kettle is equipped with discharge gate, the feed inlet with discharge gate department all are equipped with valve gate. The utility model has the advantages of: the sealing performance of promotion ensures that the reaction process is more thorough and efficient, and the reaction efficiency is greatly improved.

Description

Technical Field

[0001] This utility model relates to the field of lithium battery preparation technology, and in particular to an apparatus for synthesizing lithium sulfide. Background Technology

[0002] Since its invention, lithium-ion batteries have been widely used in portable electronic devices such as cameras, laptops, mobile phones, and power tools due to their high cycle life and high energy density. In recent years, with the continuous improvement of lithium-ion batteries, they have even been applied to the field of new energy vehicles. Currently, there is particular attention in this field to all-solid-state batteries with high safety and high energy density. Among them, inorganic solid-state batteries, mainly based on sulfide solid-state batteries, are favored by academia and the commercial community due to the advantages of their electrolytes, such as high ionic conductivity, ease of forming framework structures, and good electrochemical stability. Among sulfide solid-state electrolytes, electrolytes with lithium silver germanium mineral structures occupy an important position, especially Li6PS5X (X = Cl, Br, and I), and Cl-rich LPSC, in particular, has high ionic conductivity and shows broad application prospects in all-solid-state batteries. However, the synthesis process of LPSC materials is extremely sensitive to water and oxygen, and the precursor material (lithium sulfide) is particularly expensive, resulting in high material costs, which seriously hinders the development of all-solid-state batteries.

[0003] Lithium sulfide, a key raw material for LPSC synthesis, is currently in a critical period of cost reduction. How to produce lithium sulfide in large quantities and with high quality will be a key factor in the application of solid-state batteries. There are many methods for synthesizing lithium sulfide on the market, mainly including the reduction method, which uses carbon / hydrogen to reduce lithium sulfate at high temperatures; this method mainly involves solid-solid or gas-solid reactions; the combustion method, which involves a violent reaction between metallic lithium and elemental sulfur, prone to explosion and requiring sophisticated equipment; and the metathesis method, which involves the reaction of lithium hydroxide and hydrogen sulfide in NMP, which is more demanding in terms of environment and reaction conditions. Currently, each method has its advantages and disadvantages, but based on the future development direction of solid-state batteries, lithium sulfide has a large market demand. From the perspective of production volume and cost, the metathesis method for synthesizing lithium sulfide has significant advantages.

[0004] The metathesis method involves the reaction of lithium hydroxide and hydrogen sulfide in NMP, a three-phase gas-liquid-solid reaction. During the reaction, lithium hydroxide, NMP, and hydrogen sulfide are three different raw materials with significant differences in density, viscosity, and phase, making the actual reaction complex. Uneven gas flow into the reactor directly leads to poor mixing of the gas, solid, and liquid raw materials, thus affecting the final reaction efficiency and product quality. Furthermore, the use of hydrogen sulfide, a highly toxic and corrosive gas, imposes stringent requirements on the equipment's sealing and corrosion resistance. Utility Model Content

[0005] The technical problem to be solved by this invention is to provide an apparatus for synthesizing lithium sulfide, which improves the sealing of the reaction environment and increases the reaction efficiency.

[0006] The technical solution of this utility model to solve the above-mentioned technical problems is as follows: A device for synthesizing lithium sulfide includes an integrated reaction vessel. The top of the reaction vessel is fixedly connected to one end of an exhaust pipe. A heating mechanism is provided at the bottom of the reaction vessel. A stirring mechanism is provided inside the reaction vessel. An inclined baffle is fixedly provided on the inner wall of the middle part of the reaction vessel. The baffle is annular, and the outer wall of the baffle is fixedly connected to the inner wall of the reaction vessel. The baffle is gradually inclined downward from the outer side to its inner side. An air inlet is provided at the bottom of the reaction vessel, and the air inlet is connected to an external hydrogen sulfide gas source through a pipe. A feed inlet is provided at the top of the reaction vessel, and a discharge outlet is provided at the bottom of the reaction vessel. Valves are provided at both the feed inlet and the discharge outlet.

[0007] The beneficial effects of this utility model are as follows: This utility model adopts an integrated reaction vessel, which reduces the use of numerous connecting parts, thereby significantly improving the sealing performance and effectively avoiding the risk of gas leakage from the vessel body; by setting a heating mechanism inside the reaction vessel, internal heating is achieved, and in combination with external heating, the dual heating method can make the liquid heat more evenly, ensuring a more thorough and efficient reaction process; the setting of the baffle helps to fully contact the gas and the reactants, thereby greatly improving the reaction efficiency.

[0008] Based on the above technical solution, the present invention can be further improved as follows.

[0009] Furthermore, an aeration mechanism is fixedly installed at the bottom of the reactor, and the aeration mechanism is connected to the air inlet.

[0010] The beneficial effect of adopting the above-mentioned further solution is that the aeration mechanism can increase the contact between hydrogen sulfide gas and lithium hydroxide, thereby further improving the reaction efficiency.

[0011] Furthermore, the aeration mechanism includes an aeration main pipe, which is connected to the air inlet, and a plurality of aeration ports are evenly provided on the aeration main pipe.

[0012] The advantages of adopting the above-mentioned further scheme are: simple structure and good aeration effect.

[0013] Furthermore, the stirring mechanism includes a rotating shaft that is vertically rotatably disposed inside the reactor. The bottom end of the rotating shaft extends out of the reactor and is connected to the output shaft of a rotating motor. Multiple stirring blades are fixedly disposed on the rotating shaft.

[0014] The beneficial effect of adopting the above-mentioned further solution is that the rotating motor drives the rotating shaft to rotate circumferentially, thereby driving the stirring blades to rotate, thus achieving effective stirring inside the reaction vessel.

[0015] Furthermore, the heating mechanism is located at the center of the bottom of the reactor, the rotating shaft is rotatably located at the center of the heating mechanism, and a plurality of stirring blades are located on the outside of the heating mechanism.

[0016] The advantages of adopting the above-mentioned further solution are: saving installation space and being able to stir the area around the heating mechanism, thereby improving the heat exchange efficiency of the liquid in the reactor and thus improving the reaction effect.

[0017] Furthermore, a connecting frame is fixedly provided at the top of the rotating shaft, and a plurality of connecting rods are fixedly provided around the periphery of the connecting frame. The top of the connecting rods is fixedly connected to the connecting frame, and the bottom of the connecting rods extends toward the bottom of the reactor. The stirring blades are fixedly connected to the connecting rods.

[0018] The beneficial effect of adopting the above-mentioned further solution is that the stirring blades can be arranged around the heating mechanism through the connecting frame and connecting rod.

[0019] Furthermore, the exhaust pipe is integrally and fixedly connected to the reaction vessel.

[0020] The beneficial effect of adopting the above-mentioned further solution is that the exhaust pipe and the reactor are fixed in one piece, which further improves the sealing performance of the reactor.

[0021] Furthermore, the connection between the reactor and the exhaust pipe is a funnel-shaped structure, and the inner diameter of one end of the funnel-shaped structure connected to the reactor is larger than the inner diameter of the other end.

[0022] The beneficial effects of adopting the above-mentioned further solution are: the connection between the reactor and the exhaust pipe is a funnel-shaped structure, which on the one hand facilitates the integrated manufacturing of the reactor and the exhaust pipe, and on the other hand facilitates the discharge of excess hydrogen sulfide gas.

[0023] Furthermore, the exhaust pipe is equipped with a condenser and an exhaust gas treatment mechanism.

[0024] The beneficial effects of adopting the above-mentioned further solutions are: the condenser can recover and reuse excess hydrogen sulfide gas, and the exhaust gas treatment mechanism can ensure that no hydrogen sulfide gas is emitted and causes environmental pollution.

[0025] Furthermore, the reactor is equipped with an observation window for observing its interior.

[0026] The beneficial effect of adopting the above-mentioned further solution is that the observation window facilitates the observation of the interior of the reactor. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the structure of this utility model;

[0028] Figure 2 This is a schematic diagram of the aeration mechanism in this utility model;

[0029] Figure 3 This is a top view of the internal structure of the reactor in this utility model. The stirring mechanism is not shown in the attached drawing.

[0030] The attached diagram lists the components represented by each number as follows:

[0031] 1. Rotating motor; 2. Stirring blade; 3. Heating mechanism; 4. Baffle; 5. Feed inlet; 6. Reactor; 7. Observation window; 8. Aeration mechanism; 8-1. Aeration main pipe; 8-2. Aeration port; 9. Discharge port; 10. Exhaust pipe; 11. Condenser; 12. Tail gas treatment mechanism; 13. Rotating shaft; 14. Connecting frame; 15. Connecting rod. Detailed Implementation

[0032] The principles and features of this utility model are described below with reference to the accompanying drawings. The examples given are only for explaining this utility model and are not intended to limit the scope of this utility model.

[0033] like Figure 1 As shown, an embodiment of this utility model includes an integrated reaction vessel 6. The top of the reaction vessel 6 is fixedly connected to one end of an exhaust pipe 10. Specifically, the exhaust pipe 10 is integrally and fixedly connected to the reaction vessel 6. The connection between the reaction vessel 6 and the exhaust pipe 10 is a funnel-shaped structure, and the inner diameter of the end of the funnel-shaped structure connected to the reaction vessel 6 is larger than the inner diameter of the other end. The exhaust pipe 10 and the reaction vessel 6 are integrally fixed, which improves the sealing performance and effectively prevents gas leakage from the vessel body. The funnel-shaped structure at the connection between the reaction vessel 6 and the exhaust pipe 10 facilitates the integrated manufacturing of the reaction vessel 6 and the exhaust pipe 10, and also facilitates the discharge of excess hydrogen sulfide gas.

[0034] The bottom of the reaction vessel 6 is provided with a heating mechanism 3. In the embodiment of this utility model, the heating mechanism 3 can be a commonly used heating device in the prior art, such as a heating furnace. The reaction vessel 6 is provided with a stirring mechanism. While ensuring the uniformity of the solution in the reaction vessel 6, the stirring mechanism disperses the reaction gas as much as possible, so that it is finely and evenly distributed in the solution, thereby enhancing the reaction efficiency.

[0035] like Figure 1 , Figure 2 and Figure 3As shown in the embodiment of this utility model, the baffle 4 can be an integral annular baffle structure. The outer peripheral wall of the annular baffle structure is fixedly connected to the inner wall of the reaction vessel 6, and the inner wall of the annular baffle structure is inclined downwards, forming a channel in the middle of the annular baffle structure for excess hydrogen sulfide gas to pass through. To illustrate the relative positional relationship between the baffle 4 and the aeration mechanism 8, Figure 3 The baffle 4 in the figure is a partial cross-section. The baffle 4 not only changes the flow field inside the reactor 6 and enhances the uniformity of the liquid composition inside the reactor 6, but also maximizes the residence time of the reaction gas inside the reactor, preventing it from escaping quickly and causing incomplete reaction.

[0036] The bottom of the reactor 6 is provided with an air inlet, which is connected to an external hydrogen sulfide gas source through a pipe; the upper part of the reactor 6 is provided with a feed inlet 5, which is located above the baffle 4. The inclined baffle 4 can guide the NMP and lithium hydroxide added from the feed inlet 5 to the bottom of the reactor 6. The bottom of the reactor 6 is provided with a discharge outlet 9, and valves are provided at both the feed inlet 5 and the discharge outlet 9.

[0037] In this embodiment, an aeration mechanism 8 is fixedly installed at the bottom of the reaction vessel 6. The aeration mechanism 8 is connected to the air inlet. The aeration mechanism 8 increases the contact between hydrogen sulfide gas and lithium hydroxide, thereby further improving the reaction efficiency. Specifically, as shown... Figure 2 As shown, the aeration mechanism 8 includes an aeration main pipe 8-1, which is connected to the air inlet, and a plurality of aeration ports 8-2 are evenly provided on the aeration main pipe 8-1.

[0038] In an embodiment of this utility model, the stirring mechanism includes a rotating shaft 13 vertically rotatably disposed inside the reaction vessel 6. The bottom end of the rotating shaft 13 extends out of the reaction vessel 6 and is connected to the output shaft of the rotating motor 1. A plurality of stirring blades 2 are fixedly disposed on the rotating shaft 13. The rotating motor 1 drives the rotating shaft 13 to rotate circumferentially, thereby driving the stirring blades 2 to rotate, thereby achieving effective stirring inside the reaction vessel 6.

[0039] Furthermore, the heating mechanism 3 is located at the center of the bottom of the reactor 6, the rotating shaft 13 is rotatably located at the center of the heating mechanism 3, and multiple stirring blades 2 are located on the outside of the heating mechanism 3, which saves installation space and can stir the area around the heating mechanism 3, thereby improving the heat exchange efficiency of the liquid in the reactor 6 and thus improving the reaction effect.

[0040] In addition to being located at the center of the bottom of the reactor 6, the heating mechanism 3 can also be arranged in multiple evenly at the bottom of the reactor 6 to improve the uniformity of heating. When the heating mechanism 3 is not located at the center of the bottom of the reactor 6, multiple stirring mechanisms can be arranged as needed, or it can be determined whether to install them together with the heating mechanism 3 as needed.

[0041] A connecting frame 14 is fixedly provided on the top of the rotating shaft 13. A plurality of connecting rods 15 are fixedly provided around the periphery of the connecting frame 14. The top of the connecting rods 15 is fixedly connected to the connecting frame 14. The bottom of the connecting rods 15 extends toward the bottom of the reactor 6. The stirring blade 2 is fixedly connected to the connecting rod 15. The stirring blade 2 can be arranged around the heating mechanism 3 through the connecting frame 14 and the connecting rods 15.

[0042] In an embodiment of this utility model, in order to facilitate the treatment of unreacted hydrogen sulfide gas, the exhaust pipe 10 is provided with a condenser 11 and a tail gas treatment mechanism 12 (the specific structures of the condenser 11 and the tail gas treatment mechanism 12 are conventional technologies in the field and will not be described in detail here). The condenser 11 can recycle excess hydrogen sulfide gas, and the tail gas treatment mechanism 12 can ensure that no hydrogen sulfide gas is discharged and causes pollution to the environment.

[0043] The reactor 6 is provided with an observation window 7 for observing its interior. The observation window 7 is located on the upper part of the reactor 6, and the observation window 7 facilitates the observation of the interior of the reactor 6.

[0044] The beneficial effects of this utility model are as follows:

[0045] 1. Compared with the traditional reactor 6, the integrated design of the reactor 6 reduces the use of many connecting parts, thereby significantly improving the sealing performance and effectively avoiding the risk of leakage of the reactor body.

[0046] 2. A baffle 4 is specially added inside the reactor 6. This design helps to ensure full contact between the gas and the reactants, thereby greatly improving the reaction efficiency.

[0047] 3. The heating mechanism 3 is cleverly integrated at the center of the bottom of the reactor 6. Compared with the traditional reactor 6 which is only heated from the outside, this dual heating method of the inside and outside can make the liquid heat more evenly, ensuring a more thorough and efficient reaction process.

[0048] In the description of this utility model, it should be understood that the terms "center", "length", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "inner", "outer", "circumferential", "circumferential", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the system or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0049] In the description of this utility model, "multiple" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0050] In this utility model, unless otherwise explicitly specified and limited, the terms "installation," "connection," "joining," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.

[0051] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0052] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. An apparatus for synthesizing lithium sulfide, characterized in that, The reactor includes an integrated reactor (6), the top of which is fixedly connected to one end of an exhaust pipe (10). A heating mechanism (3) is provided at the bottom of the reactor (6). A stirring mechanism is provided inside the reactor (6). An inclined baffle (4) is fixedly provided on the inner wall of the middle part of the reactor (6). The baffle (4) is annular. The outer peripheral wall of the baffle (4) is fixedly connected to the inner wall of the reactor (6). The baffle (4) is gradually inclined downward from the outside to the inside. An air inlet is provided at the bottom of the reactor (6). The air inlet is connected to an external hydrogen sulfide gas source through a pipe. A feed inlet (5) is provided at the top of the reactor (6). An outlet (9) is provided at the bottom of the reactor (6). Valves are provided at both the feed inlet (5) and the outlet (9).

2. The apparatus for synthesizing lithium sulfide according to claim 1, characterized in that, An aeration mechanism (8) is fixedly installed at the bottom of the reactor (6), and the aeration mechanism (8) is connected to the air inlet.

3. The apparatus for synthesizing lithium sulfide according to claim 2, characterized in that, The aeration mechanism (8) includes an aeration main pipe (8-1), which is connected to the air inlet, and a plurality of aeration ports (8-2) are evenly provided on the aeration main pipe (8-1).

4. The apparatus for synthesizing lithium sulfide according to claim 1, characterized in that, The stirring mechanism includes a rotating shaft (13) that is vertically rotatably installed inside the reactor (6). The bottom end of the rotating shaft (13) extends out of the reactor (6) and is connected to the output shaft of the rotating motor (1). Multiple stirring blades (2) are fixedly provided on the rotating shaft (13).

5. The apparatus for synthesizing lithium sulfide according to claim 4, characterized in that, The heating mechanism (3) is located at the center of the bottom of the reactor (6), the rotating shaft (13) is rotatably located at the center of the heating mechanism (3), and a plurality of stirring blades (2) are located on the outside of the heating mechanism (3).

6. The apparatus for synthesizing lithium sulfide according to claim 5, characterized in that, A connecting frame (14) is fixedly provided on the top of the rotating shaft (13). A plurality of connecting rods (15) are fixedly provided around the periphery of the connecting frame (14). The top of the connecting rod (15) is fixedly connected to the connecting frame (14). The bottom of the connecting rod (15) extends toward the bottom of the reactor (6). The stirring blade (2) is fixedly connected to the connecting rod (15).

7. The apparatus for synthesizing lithium sulfide according to claim 1, characterized in that, The exhaust pipe (10) is integrally and fixedly connected to the reaction vessel (6).

8. The apparatus for synthesizing lithium sulfide according to claim 7, characterized in that, The connection between the reactor (6) and the exhaust pipe (10) is a horn-shaped structure, and the inner diameter of one end of the horn-shaped structure connected to the reactor (6) is larger than the inner diameter of the other end.

9. An apparatus for synthesizing lithium sulfide according to any one of claims 1 to 8, characterized in that, The exhaust pipe (10) is equipped with a condenser (11) and an exhaust gas treatment mechanism (12).

10. An apparatus for synthesizing lithium sulfide according to any one of claims 1 to 8, characterized in that, The reactor (6) is provided with an observation window (7) for observing its interior.

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