Lithium sulfide manufacturing apparatus and method for manufacturing lithium sulfide

Abstract

To provide a device for producing lithium sulfide with high efficiency and stability.SOLUTION: A device for producing lithium sulfide according to the present invention comprises: a reactor 3 having a lithium sulfide filling part 2 inside; a jacket heater 4 that is heating means of heating lithium sulfide; and a hydrogen sulfide supply pipe 5 that is a hydrogen sulfide supply member connected to the reactor 3. The inside of the reactor 3 is provided with an inverted funnel-like lithium sulfide collecting member 6 above the lithium sulfide filling part 2.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present invention relates to an apparatus for producing lithium sulfide and a method for producing lithium sulfide. [Background technology]

[0002] A method for producing lithium sulfide is known in which hydrogen sulfide gas is reacted with lithium hydroxide. Examples of techniques related to such methods for producing lithium sulfide include those described in Patent Document 1 (JP 2016-150860 A). [Prior art documents] [Patent documents]

[0003] [Patent Document 1] JP 2016-150860 A Summary of the Invention [Problem to be solved by the invention]

[0004] However, with the lithium sulfide production techniques disclosed in Patent Document 1 and the like, it has been difficult to achieve sufficiently high production efficiency.

[0005] The present invention has been made in consideration of the above circumstances, and an object of the present invention is to provide an apparatus for manufacturing lithium sulfide that can produce lithium sulfide with high efficiency. [Means for solving the problem]

[0006] According to the present invention, An apparatus for producing lithium sulfide by reacting hydrogen sulfide with lithium hydroxide, comprising: A reactor having a lithium hydroxide filled portion therein; A heating means for heating the lithium hydroxide; A hydrogen sulfide supply unit connected to the reactor; Equipped with Inside the reactor, an inverted funnel-shaped lithium sulfide recovery member is provided above the lithium hydroxide-filled part, thereby providing an apparatus for producing lithium sulfide.

[0007] Furthermore, according to the present invention, there is provided a method for producing lithium sulfide, which comprises reacting hydrogen sulfide gas with lithium hydroxide using the above-described apparatus for producing lithium sulfide. Effect of the Invention

[0008] According to the present invention, it is possible to provide an apparatus for manufacturing lithium sulfide with excellent manufacturing efficiency. [Brief description of the drawings]

[0009] [Figure 1] FIG. 1 is a vertical sectional view of an example of an apparatus for manufacturing lithium sulfide according to an embodiment of the present invention. [Diagram 2] 3A and 3B are a longitudinal sectional view and a perspective view of an example of an inverted funnel-shaped lithium sulfide recovery member of the lithium sulfide manufacturing apparatus of the present embodiment. [Diagram 3] FIG. 2 is a top view of a lithium hydroxide support member of the lithium sulfide manufacturing apparatus of the present embodiment. [Figure 4] FIG. 2 is a vertical sectional view of another example of the apparatus for manufacturing lithium sulfide according to the present embodiment. [Diagram 5] FIG. 2 is a perspective view showing a specific example of an inverted funnel-shaped lithium sulfide recovery member of the lithium sulfide manufacturing apparatus of the present embodiment. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0010] Hereinafter, an embodiment of the present invention will be described with reference to the drawings. In all the drawings, similar components are denoted by the same reference numerals, and the description thereof will be omitted as appropriate.

[0011] [First embodiment] An example of an apparatus for producing lithium sulfide according to the present embodiment will be described with reference to FIGS. 1 to 3.

[0012] Fig. 1 is a longitudinal sectional view of an apparatus for manufacturing lithium sulfide 1. Fig. 2a is a longitudinal sectional view of an inverted funnel-shaped lithium sulfide recovery member 6 provided in the apparatus for manufacturing lithium sulfide 1 of the present embodiment. Fig. 2b is a perspective view of the inverted funnel-shaped lithium sulfide recovery member 6 provided in the apparatus for manufacturing lithium sulfide 1 of the present embodiment. Fig. 3 is a top view of a lithium hydroxide support member 7 provided in the apparatus for manufacturing lithium sulfide 1.

[0013] The lithium sulfide manufacturing apparatus 1 includes a reactor 3 having a lithium hydroxide-filled section 2 therein, a jacket heater 4 serving as a heating means for heating the lithium hydroxide, and a hydrogen sulfide supply pipe 5 serving as a hydrogen sulfide supply member connected to the reactor 3. Inside the reactor 3, an inverted funnel-shaped lithium sulfide recovery member 6 is provided above the lithium hydroxide-filled section 2.

[0014] In the lithium sulfide manufacturing apparatus 1 of the present embodiment, since the inverted funnel-shaped lithium sulfide recovery member 6 is provided above the reactor 3, lithium sulfide produced in the reactor 3 can be recovered by sucking it through the legs of the inverted funnel-shaped lithium sulfide recovery member 6. This makes it possible to recover lithium sulfide without dismantling the lithium sulfide manufacturing apparatus 1, increasing the lithium sulfide recovery efficiency and enabling lithium sulfide to be produced with high production efficiency.

[0015] Hereinafter, the configuration of each part of the apparatus for manufacturing lithium sulfide according to the present embodiment will be described.

[0016] (Reactor 3) Inside the reactor 3, lithium hydroxide (solid) reacts with hydrogen sulfide gas to produce lithium sulfide (solid).

[0017] A hydrogen sulfide supply pipe 5 is connected to the reactor 3, and hydrogen sulfide is supplied from the hydrogen sulfide supply pipe 5.

[0018] The reactor 3 is also provided with a lithium hydroxide support member 7, and the space surrounded by the lithium hydroxide support member 7 and the inner wall of the reactor 3 is referred to as a lithium hydroxide filled section 2.

[0019] Lithium hydroxide (not shown) is placed on the lithium hydroxide supporting member 7 .

[0020] The hydrogen sulfide supply pipe 5 is preferably positioned below the lithium hydroxide support member 7. This is because hydrogen sulfide gas is supplied from below to the lithium hydroxide support member 7, and thereby passes toward the top of the reactor 3, where it comes into contact with the lithium hydroxide filled in the lithium hydroxide filling section 2, efficiently discharging water (water vapor), a by-product having a smaller specific gravity than hydrogen sulfide gas. In addition, fresh hydrogen sulfide gas is constantly supplied by continuously passing hydrogen sulfide gas toward the top of the reactor 3.

[0021] 3, the lithium hydroxide support member 7 is preferably provided with a plurality of communication holes 171. This is because the hydrogen sulfide gas supplied from the hydrogen sulfide supply pipe 5 is efficiently supplied to the lithium hydroxide filled section 2 through the communication holes 171.

[0022] The hydrogen sulfide gas supplied from hydrogen sulfide supply pipe 5 comes into contact with the surface of lithium hydroxide (solid) filled in lithium hydroxide filled section 2.

[0023] It is believed that the reaction shown in equation (1) below occurs on the surface of lithium hydroxide (solid). 2LiOH+H2S→Li2S+2H2O(1)

[0024] In the lithium hydroxide-filled section 2 inside the reactor 3, the lithium hydroxide is preferably filled in layers so that the lithium hydroxide filled in layers is in contact with the inner wall surface of the reactor 3. This is because heating can be achieved by heat transfer from the inner wall surface of the lithium hydroxide-filled section 2, thereby increasing the heating efficiency.

[0025] From the viewpoint of promoting the above reaction and preventing the lithium hydroxide from melting, the temperature of the lithium hydroxide-filled part 2 is usually adjusted to 100 to 445° C., and preferably 130 to 410° C. The temperature of the lithium hydroxide-filled part 2 is usually measured at the horizontal center of the lithium hydroxide-filled part 2.

[0026] Examples of the material of the reactor 3 include metals and ceramics, but it is preferable that the material be sulfur-resistant. Examples of the sulfur-resistant material include metal-based sulfur-resistant materials such as stainless steel and aluminum, and ceramic-based sulfur-resistant materials such as quartz, boron nitride, aluminum nitride, and silicon nitride.

[0027] The inner surface of the reactor 3 is preferably subjected to anti-sulfurization treatment.

[0028] Examples of the anti-sulfuration treatment include plating with a metal or alloy having high anti-sulfuration performance, such as tin plating, chromium plating, gold plating, hot-dip aluminum plating, or alloy plating containing these metals.

[0029] Alternatively, a metal diffusion infiltration treatment may be used as a means for sulfur resistance treatment. It is known that when a metal diffusion infiltration layer is formed on the surface of a treated object by subjecting the treated object to a metal diffusion infiltration treatment, the sulfur resistance performance is improved. For example, a calorizing treatment can be used, which is a diffusion and infiltration treatment of aluminum. In the calorizing treatment, the workpiece is embedded in a steel case together with a mixture consisting of Fe-Al alloy powder and NH4Cl powder, the case is sealed, and it is heated in a furnace to form an aluminum diffusion infiltration layer on the surface of the workpiece, which improves the sulfurization resistance of the workpiece.

[0030] (Jacket Heater 4) In this embodiment, a jacket heater 4 is used as a heating means for heating the lithium hydroxide.

[0031] That is, the jacket heater 4 heats the lithium hydroxide support member 7 and the space above the lithium hydroxide support member 7. This heats the lithium hydroxide filled in the lithium hydroxide filling section 2, thereby accelerating the lithium sulfide production reaction.

[0032] The temperature of the jacket heater 4 is configured to be able to adjust the temperature of the lithium hydroxide-filled section 2 to the above-mentioned temperature range. Since the required heating temperature varies depending on the diameter of the liquid lithium hydroxide-filled section 2 and the amount of catalyst filled, the temperature range of the jacket heater 4 is not particularly limited, but is preferably 100 to 445°C, and more preferably 130 to 410°C.

[0033] In addition, in this embodiment, the jacket heater 4 is used as the heating means, but the present invention is not limited to this, and any heating means capable of heating lithium hydroxide may be used. For example, a method of introducing heated hydrogen sulfide gas, a high-frequency induction heating device, etc. may also be used.

[0034] (Hydrogen sulfide supply pipe 5) The hydrogen sulfide supply pipe 5 is a member for supplying hydrogen sulfide gas to the reactor 3 .

[0035] The hydrogen sulfide supply pipe 5 is preferably positioned below the lithium hydroxide support member 7. This is because hydrogen sulfide gas is supplied from below to the lithium hydroxide support member 7, and thereby passes toward the top of the reactor 3, where it comes into contact with the lithium hydroxide filled in the lithium hydroxide filling section 2, efficiently discharging water (water vapor), a by-product having a smaller specific gravity than hydrogen sulfide gas. In addition, fresh hydrogen sulfide gas is constantly supplied by continuously passing hydrogen sulfide gas toward the top of the reactor 3.

[0036] 1, the hydrogen sulfide supply pipe 5 may have a hydrogen sulfide supply regulating valve 8 that regulates the amount of hydrogen sulfide gas supplied. The amount of hydrogen sulfide supplied can be controlled by adjusting the opening and closing of the hydrogen sulfide supply regulating valve 8, which is preferable from the viewpoint of controlling the lithium sulfide production reaction carried out in the reactor 3.

[0037] As the material for the hydrogen sulfide supply pipe 5, the materials mentioned above as the material for the reactor 3 can be used.

[0038] The hydrogen sulfide supply pipe 5 preferably has an inner surface that is anti-sulfurized. As a means for anti-sulfurizing, the method described above as a method for anti-sulfurizing the inner surface of the reactor 3 can be used.

[0039] In addition, in this embodiment, the hydrogen sulfide supply pipe 5 is used as the hydrogen sulfide supply member, but the present invention is not limited to this and any hydrogen sulfide supply member capable of supplying hydrogen sulfide gas to the reactor 3 may be used.

[0040] (Inverted funnel-shaped lithium sulfide recovery component 6) The inverted funnel-shaped lithium sulfide recovery member 6 is an inverted funnel-shaped member provided above the lithium hydroxide loading portion, and includes legs 61 and a main body 62. The main body 62 is provided with an opening 63.

[0041] In the inverted funnel-shaped lithium sulfide recovery member 6, the leg parts 61 of the inverted funnel-shaped member 6 function as a lithium sulfide recovery part. That is, lithium sulfide is recovered by connecting a recovery device to the leg parts 61, which are the lithium sulfide recovery parts. The presence of the inverted funnel-shaped lithium sulfide recovery member 6 makes it possible to recover lithium sulfide without dismantling the lithium sulfide manufacturing apparatus 1, thereby improving the lithium sulfide recovery efficiency.

[0042] Any recovery device can be used. For example, when a suction type recovery device is used, a suction member such as a suction tube is connected to the leg 61, and lithium sulfide is collected by being sucked into the suction type recovery device through the suction member. In this case, a filter may be provided in the suction member.

[0043] Since the inverted funnel-shaped lithium sulfide recovery member 6 has an inverted funnel shape, the inner diameter of the opening 63 is larger than the inner diameter of the leg portion 61. Therefore, since a wide area can be sucked by the opening 63 having a large inner diameter, lithium sulfide in the reactor 3 can be recovered more efficiently.

[0044] In the lithium sulfide manufacturing apparatus 1 of this embodiment, the legs 61 of the inverted funnel-shaped lithium sulfide recovery member 6 make it possible to communicate the upper space with the lower space of the inverted funnel-shaped lithium sulfide recovery member 6. In this way, water (water vapor) which is a by-product of the lithium sulfide production reaction and unreacted hydrogen sulfide gas move to the upper space of the inverted funnel-shaped lithium sulfide recovery member 6 and are recovered from the gas recovery pipe 10.

[0045] The inverted funnel-shaped lithium sulfide recovery member 6 preferably also functions as an inlet for lithium hydroxide.

[0046] When the inverted funnel-shaped lithium sulfide recovery member 6 also functions as an introduction portion for lithium hydroxide, lithium hydroxide is charged from the leg portion 61 of the inverted funnel-shaped lithium sulfide recovery member 6. In this case, the inner wall of the main body portion 62 protects against dust generated when charging lithium hydroxide, so that charging of lithium hydroxide can be performed more efficiently.

[0047] The inverted funnel-shaped lithium sulfide recovery member 6 is preferably provided so as to be movable up and down. This allows the inverted funnel-shaped lithium sulfide recovery member 6 to advance to the vicinity of the bottom of the reactor 3, thereby enabling efficient recovery of lithium sulfide.

[0048] The inverted funnel-shaped lithium sulfide recovery member 6 is preferably disposed so as to provide a gap (clearance) between it and the inner wall of the reactor 3. If a gap is provided between it and the inner wall of the reactor 3, when the volume of lithium sulfide filled in the reactor 3 decreases due to recovery, the inverted funnel-shaped lithium sulfide recovery member 6 can move downward accordingly.

[0049] The shape of the inverted funnel-shaped lithium sulfide recovery member 6 is not particularly limited as long as it is inverted funnel-shaped. From the viewpoint of improving the lithium sulfide recovery efficiency, however, the ratio (L1 / R1) of the inner diameter R1 of the leg portion 61 to the length L1 of the leg portion 61 is preferably 1.0 to 10, and more preferably 1.6 to 2.5.

[0050] The shape of the inverted funnel-shaped lithium sulfide recovery member 6 is not particularly limited as long as it is inverted funnel-shaped. From the viewpoint of improving the lithium sulfide recovery efficiency, however, the ratio (R2 / R1) of the inner diameter R1 of the leg portion 61 to the inner diameter R2 of the opening 63 is preferably 2.0 to 20, and more preferably 4.0 to 12.

[0051] As the material of the inverted funnel-shaped lithium sulfide recovery member 6, the materials mentioned above as the material of the reactor 3 can be used.

[0052] Furthermore, the inner wall of the inverted funnel-shaped lithium sulfide recovery member 6 may be provided with grooves or unevenness. By providing the grooves or unevenness, lithium sulfide is less likely to adhere to the inner wall of the inverted funnel-shaped lithium sulfide recovery member 6 during lithium sulfide recovery, making it possible to perform recovery more efficiently. Furthermore, the inner wall of the inverted funnel-shaped lithium sulfide recovery member 6 can be subjected to an antistatic treatment to make it less likely for lithium sulfide to adhere.

[0053] The main body of the inverted funnel-shaped lithium sulfide recovery member 6 may be a combination of a conical main body 63a and a leg 61a as shown in FIG. 5a, a combination of a hemispherical main body 63b and a leg 61b as shown in FIG. 5b, or a combination of a cylindrical main body 63c and a leg 61c as shown in FIG. 5c.

[0054] When the lithium sulfide manufacturing apparatus 1 of the present embodiment is provided with the temperature sensor 9, the temperature sensor 9 can be inserted into the leg portion 61 of the inverted funnel-shaped lithium sulfide recovery member 6 and connected to the lithium hydroxide loading portion 2. In this case, by forming a gap between the temperature sensor 9 and the inner wall of the leg portion 61 of the inverted funnel-shaped lithium sulfide recovery member 6, it is possible to communicate the upper space and the lower space of the inverted funnel-shaped lithium sulfide recovery member 6 through the gap.

[0055] (Lithium hydroxide support member 7) The lithium hydroxide support member 7 is a member for placing a lithium hydroxide support member thereon.

[0056] As described above, in order to enable heating by heat transfer from the inner wall surface of reactor 3, it is preferable that the lithium hydroxide is packed in a layer so as to be in contact with the inner wall of lithium hydroxide-filled section 2. Therefore, in order to enable lithium hydroxide to be placed in this manner, the lithium hydroxide support member 7 is preferably arranged so as to be in contact with the inner wall of lithium hydroxide-filled section 2.

[0057] 3, the lithium hydroxide support member 7 is preferably provided with a plurality of communication holes 171. By providing the heat insulating member with a plurality of communication holes 171, hydrogen sulfide supplied from the hydrogen sulfide supply pipe 5 can be efficiently supplied to the lithium hydroxide filled section 2 through the plurality of communication holes 171.

[0058] As the material of the lithium hydroxide support member 7, the materials mentioned above as the material of the reactor 3 can be used.

[0059] The shape of the lithium hydroxide support member 7 is not particularly limited as long as it allows lithium hydroxide to be placed thereon, but as described above, it is preferable that the lithium hydroxide support member 7 is provided with a plurality of communication holes 171. For example, one or more types of porous materials selected from metal meshes such as stainless steel mesh and aluminum mesh, punched metals such as stainless steel punching and aluminum punching, and expanded metals such as stainless steel expand and aluminum expand can be used.

[0060] If necessary, the lithium hydroxide support member 7 may be made of two or more sheets of the above-mentioned porous material stacked together.

[0061] The diameter of the communication hole 171 provided in the lithium hydroxide support member 7 depends on the diameter of the lithium hydroxide to be placed, but is usually 26 μm or more and 300 μm or less, and preferably 45 μm or more and 154 μm or less.

[0062] (Gas exhaust pipe 10) The gas exhaust pipe 10 is a member for discharging, to the outside of the reactor 3, exhaust gas that contains unreacted hydrogen sulfide and water produced by the reaction between hydrogen sulfide gas and lithium hydroxide.

[0063] It is preferable that the gas exhaust pipe 10 is positioned above the lithium hydroxide support member 7. The by-product water (water vapor) and unreacted hydrogen sulfide gas are vented toward the top of the reactor, and therefore, providing the gas exhaust pipe 10 at the top improves the efficiency of gas exhaust. By improving the efficiency of gas exhaust, fresh hydrogen sulfide gas is constantly supplied.

[0064] It is preferable that the gas exhaust pipe 10 is provided with a cooling section for capturing water generated by the reaction between hydrogen sulfide gas and lithium hydroxide. When the reaction between hydrogen sulfide gas and lithium hydroxide is completed, the water generated during the production of lithium sulfide will no longer condense in the cooling section. In other words, the progress of the lithium sulfide production reaction can be monitored by the amount of condensed water.

[0065] (Temperature Sensor 9) The temperature sensor 9 is a member for measuring the temperature inside the reactor 3. For example, by measuring the temperature inside the reactor 3 with the temperature sensor 9 and adjusting the heating based on the measurement result, it becomes possible to control the production of lithium sulfide more precisely.

[0066] [Second embodiment] The apparatus for manufacturing lithium sulfide of the present embodiment may further include a heat transfer member 22 arranged in contact with or in the vicinity of the bottom surface of the lithium hydroxide loading section 2. Fig. 4 is a schematic diagram showing a vertical cross section of an apparatus 21 for manufacturing lithium sulfide configured as above. By providing the heat transfer member 22 at the bottom of the lithium hydroxide-filled section 2, heat from the jacket heater 4 covering the outside of the reactor 3 is more easily transferred in the horizontal direction of the cross section of the lithium hydroxide-filled section 2, improving the thermal uniformity of the lithium hydroxide-filled section 2 in the horizontal direction.

[0067] The heat transfer member 22 is preferably disposed so as to be in contact with the inner wall of the portion filled with lithium hydroxide, in order to transfer heat from the jacket heater 4 covering the outside of the reactor 3 more efficiently.

[0068] It is preferable that a plurality of communication holes are provided in the heat transfer member 22. This is because by providing a plurality of communication holes in the heat transfer member, hydrogen sulfide supplied from the hydrogen sulfide supply pipe 5 can be efficiently supplied to the lithium hydroxide filled section 2 through the plurality of communication holes.

[0069] The material of the heat transfer member 22 is not particularly limited, and the materials mentioned above as the materials of the reactor 3 can be used, but it is preferable to use a material having excellent sulfidation resistance and thermal conductivity, such as aluminum, an aluminum alloy, aluminum nitride, silicon nitride, etc.

[0070] Furthermore, the shape of the heat transfer member 22 is not particularly limited, but for example, one or more types of porous plates selected from stainless steel or aluminum plates with a thickness of 20 mm or more and having communicating holes can be used.

[0071] If necessary, the heat transfer member 22 may be made of two or more sheets of the above-mentioned porous material stacked together.

[0072] The area ratio of the communicating holes provided in the heat transfer member 22 is typically 0.2% or more and 50% or less, and preferably 0.5% or more and 40% or less, from the viewpoint of a balance between improving heat transfer efficiency and improving the contact efficiency between the sulfur vapor and the catalyst.

[0073] The diameter of the communication hole provided in the heat transfer member 22 is usually 26 μm or more and 10,000 μm or less, and preferably 45 μm or more and 5,000 μm or less.

[0074] [Variations] The apparatus for manufacturing lithium sulfide of the present embodiment may include components other than the components described above.

[0075] Moreover, in the apparatus for manufacturing lithium sulfide according to the present embodiment, each part may be integrally formed.

[0076] [Lithium sulfide manufacturing process] A lithium sulfide manufacturing process using the lithium sulfide manufacturing apparatus 1 of this embodiment will be described.

[0077] First, lithium hydroxide is filled into lithium hydroxide-filled section 2, and lithium hydroxide-filled section 2 filled with lithium hydroxide is heated by jacket heater 4, which is a heating means.

[0078] In the lithium sulfide manufacturing apparatus 1 of the present embodiment, it is preferable that the inverted funnel-shaped lithium sulfide recovery member 6 also functions as an introduction portion for lithium hydroxide, in which case lithium hydroxide is charged from the leg portion 61 of the inverted funnel-shaped lithium sulfide recovery member 6. In this case, dust generated during charging of lithium hydroxide is prevented by the inner wall of the opening 63, so that charging of lithium hydroxide can be performed more efficiently.

[0079] Next, hydrogen sulfide gas is supplied to lithium hydroxide charging section 2, and the hydrogen sulfide gas is brought into contact with the lithium hydroxide, causing the lithium hydroxide and the hydrogen sulfide gas to react with each other to produce lithium sulfide.

[0080] In the lithium sulfide manufacturing process using the lithium sulfide manufacturing apparatus 1, the temperature of the lithium hydroxide-filled section 2 is preferably 150° C. or higher in the entire region, more preferably 170° C. or higher, and even more preferably 200° C. or higher. When the temperature of the catalyst-filled section is equal to or higher than the above-mentioned lower limit in the entire region, the reaction rate between hydrogen sulfide gas and lithium hydroxide can be further improved.

[0081] In the lithium sulfide manufacturing process using the lithium sulfide manufacturing apparatus 1, the temperature of the lithium hydroxide-filled section 2 is preferably 445°C or less in all regions, more preferably 430°C or less, and even more preferably 410°C or less. When the temperature of the catalyst-filled section is equal to or less than the upper limit value in all regions, the lithium hydroxide can be prevented from melting, and therefore, the lithium hydroxide can be prevented from fusing with each other to form a mass. This makes it possible to more effectively proceed with the reaction between the reaction gas and the lithium hydroxide.

[0082] The d50 in the weight-based particle size distribution of lithium hydroxide measured by a laser diffraction scattering particle size distribution measurement method is preferably 1.5 mm or less, more preferably 1.0 mm or less. When the d50 is equal to or less than the upper limit, the contact area between the lithium hydroxide and the reaction gas increases, accelerating the reaction, and the amount of unreacted raw material in the obtained lithium sulfide can be further reduced. As a result, lithium sulfide with higher purity can be obtained. In addition, the d50 in the weight-based particle size distribution of lithium hydroxide measured by a laser diffraction scattering particle size distribution measurement method is preferably 0.1 mm or more, more preferably 0.2 mm or more. When the average particle size is equal to or more than the above lower limit, water generated in the reaction system can be prevented from adhering to the lithium sulfide particles and causing the particles to stick. In addition, it is possible to suppress the lithium hydroxide and the obtained lithium sulfide from being discharged together with the reaction gas, so that the exhaust gas treatment can be simplified. In addition, it is possible to suppress the lithium hydroxide and the obtained lithium sulfide from being scattered by the reaction gas, so that the yield of lithium sulfide can be improved.

[0083] It is preferable to previously remove water of crystallization from lithium hydroxide and dry the adhering water. This makes it possible to prevent lithium hydroxide from agglomerating and to prevent the generation of hydrosulfides, so that the reaction between hydrogen sulfide gas and lithium hydroxide can proceed more effectively. Examples of methods for dehydrating and drying lithium hydroxide include a method of heating in the atmosphere, a method of heating while flowing a gas such as hydrogen, nitrogen, or argon gas, and a method of heating under reduced pressure.

[0084] The hydrogen sulfide gas may be a commercially available product filled in a gas cylinder or the like, or may be produced in a hydrogen sulfide production apparatus connected upstream of the lithium sulfide production apparatus 1. When a hydrogen sulfide production device is connected upstream of the lithium sulfide production device 1, it is possible to generate hydrogen sulfide gas in the amount necessary for the production of lithium sulfide, eliminating the need to store hydrogen sulfide gas separately. In addition, since hydrogen sulfide gas can be generated as needed, high-purity hydrogen sulfide gas that has not deteriorated over time can be used in the reaction.

[0085] In the lithium sulfide manufacturing apparatus 1 of the present embodiment, since the inverted funnel-shaped lithium sulfide recovery member 6 is provided above the reactor 3, lithium sulfide generated in the reactor 3 can be recovered by sucking it through the legs 61 of the inverted funnel-shaped lithium sulfide recovery member 6. This makes it possible to recover lithium sulfide without dismantling the lithium sulfide manufacturing apparatus 1, increasing the lithium sulfide recovery efficiency and enabling lithium sulfide to be produced with high production efficiency.

[0086] In the lithium sulfide manufacturing apparatus 1 of the present embodiment, it is preferable that the inverted funnel-shaped lithium sulfide recovery member 6 is provided so as to be movable up and down. This allows the inverted funnel-shaped lithium sulfide recovery member 6 to advance to the vicinity of the bottom of the reactor 3, thereby enabling efficient recovery of lithium sulfide.

[0087] Lithium sulfide obtained by the manufacturing process using the lithium sulfide manufacturing apparatus 1 can be suitably used, for example, as a positive electrode active material, a negative electrode active material, a solid electrolyte material, or an intermediate raw material for chemicals for batteries.

[0088] Although the embodiments of the present invention have been described above, these are merely examples of the present invention, and various configurations other than those described above can also be adopted. [Explanation of symbols]

[0089] 1 Lithium sulfide manufacturing equipment 2 Lithium hydroxide filling section 3. Reactor 4 Jacket Heater 5 Hydrogen sulfide supply pipe 6 Inverted funnel-shaped lithium sulfide recovery component 7 Lithium hydroxide support member 8 Hydrogen sulfide supply control valve 9 Temperature Sensor 10 Gas exhaust pipe 21 Lithium sulfide manufacturing equipment 22 Heat transfer materials 61 Legs 62 Main body 63 Opening 61a Legs 62a Cone-shaped body 61b Legs 62b Hemispherical body part 61c Legs 62c Cylindrical body 171 Communication hole

Claims

1. An apparatus for producing lithium sulfide by reacting hydrogen sulfide with lithium hydroxide, comprising: A reactor having a lithium hydroxide filled portion therein; A heating means for heating the lithium hydroxide; A hydrogen sulfide supply connected to the reactor; Equipped with the reactor is provided with an inverted funnel-shaped lithium sulfide recovery member above the lithium hydroxide packed section.

2. The lithium sulfide manufacturing apparatus according to claim 1, The apparatus for manufacturing lithium sulfide, wherein the inverted funnel-shaped lithium sulfide recovery member also serves as a lithium hydroxide supply member.

3. The lithium sulfide manufacturing apparatus according to claim 1 or 2, The inverted funnel-shaped lithium sulfide recovery member is provided so as to be movable forward and backward in the vertical direction.

4. The apparatus for producing lithium sulfide according to any one of claims 1 to 3, The apparatus for manufacturing lithium sulfide further comprises a heat transfer member arranged in contact with or in proximity to a bottom surface of the lithium hydroxide filled section.

5. The lithium sulfide manufacturing apparatus according to any one of claims 1 to 4, Lithium sulfide manufacturing equipment with an anti-sulfurized inner surface.

6. A method for producing lithium sulfide, comprising reacting hydrogen sulfide gas with lithium hydroxide using the apparatus for producing lithium sulfide according to any one of claims 1 to 5.

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