Lithium sulfide preparation device

Abstract

The utility model belongs to the field of lithium sulfide preparation devices, and discloses a lithium sulfide preparation device. The lithium sulfide preparation device comprises a reaction kettle, a gas return pipe, a moisture detector and a gas dryer, the reaction kettle is provided with a reaction cavity, a gas inlet pipe, a tail gas pipe and a discharge hole; one end of the gas return pipe is communicated with the tail gas pipe, and the other end of the gas return pipe is communicated with the gas inlet pipe, so that the hydrogen sulfide which is not completely reacted in the tail gas is recycled and can be reguided back to the reaction cavity, and the recycling rate of the hydrogen sulfide is increased. The moisture detector is arranged at the gas inlet end of the gas return pipe, the gas dryer is arranged at the gas outlet end of the gas return pipe, and reaction tail gas sequentially passes through the moisture detector and the gas dryer and then enters the gas inlet pipe again. And the gas dryer can remove moisture in the tail gas to ensure that the gas introduced into the gas inlet pipe is in a dry state, so that the reverse reaction of lithium sulfide is prevented, and the purity and yield of the product are further improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of lithium sulfide preparation devices, and more specifically relates to a lithium sulfide preparation device. Background Art

[0002] In the current field of chemical synthesis, lithium sulfide, as an important inorganic compound, has shown broad application potential in various fields such as battery materials, photovoltaic materials, and catalysts. Currently, the synthesis methods of lithium sulfide mainly include ball milling, solvent method, high temperature and high pressure method, direct carbon composite method, and hydrogen sulfide gas-solid synthesis method.

[0003] The ball milling method promotes the mixing and reaction between reactants through the action of mechanical force, but this method often requires a high energy input and a long reaction cycle, resulting in low production efficiency. Although the solvent method has improved the selectivity and uniformity of the reaction to a certain extent, the organic solvents used are often flammable and explosive, which not only increases the safety risks in the production process, but also places higher demands on subsequent environmental treatment. Due to the extreme reaction conditions, the high temperature and high pressure method not only consumes a lot of energy, but also has strict requirements on the high pressure and high temperature resistance of the equipment, limiting its possibility of large-scale industrial application. The direct carbon composite method attempts to introduce carbonaceous materials as reducing agents in order to achieve the synthesis of lithium sulfide at a lower temperature. However, this method still faces problems such as low conversion rate and difficult to control product purity in actual operation, which affects its actual application effect. In contrast, the hydrogen sulfide gas-solid synthesis method was once regarded as a potential synthesis method due to its relatively low reaction temperature and high conversion rate.

[0004] However, the hydrogen sulfide gas-solid synthesis method also faces challenges in practical application. On the one hand, the reaction process is prone to reverse reaction, that is, the generated lithium sulfide may decompose back into hydrogen sulfide and lithium at high temperature, which not only reduces the yield of the product but also increases the complexity of the reaction. On the other hand, hydrogen sulfide gas itself is toxic, and the reaction exhaust contains incompletely reacted hydrogen sulfide and other harmful gases, which puts great pressure on the exhaust gas treatment system, increasing environmental risks and production costs. Utility Model Content

[0005] The purpose of the embodiments of the present application is to provide a lithium sulfide preparation device to solve the technical problems in the prior art of preparing lithium sulfide by hydrogen sulfide gas-solid synthesis method, such as the easy occurrence of reverse reaction and insufficient hydrogen sulfide reaction.

[0006] To achieve the above objectives, the technical solution adopted in this application is:

[0007] Provided is a lithium sulfide preparation device, comprising:

[0008] A reactor having a reaction chamber, an air inlet pipe, an exhaust pipe and a discharge port;

[0009] an air return pipe, one end of which is connected to the tail pipe and the other end of which is connected to the air intake pipe;

[0010] A moisture detector is provided at the air inlet end of the return air pipe, and is used to detect the water content of the exhaust gas in the exhaust pipe;

[0011] A gas dryer is provided at the gas outlet end of the return gas pipe, and is used to dry the gas entering the gas inlet pipe;

[0012] The tail gas discharged from the reaction chamber passes through the moisture detector and the gas dryer in sequence and then re-enters the air inlet pipe.

[0013] As a further improvement of the above technical solution:

[0014] Optionally, the lithium sulfide preparation device includes a return air booster, which is provided at the gas outlet end of the return air pipe, and the return air booster is used to boost the pressure of the dried gas in the return air pipe to be consistent with the gas pressure in the inlet pipe.

[0015] Optionally, the lithium sulfide preparation device includes a heater, which is used to heat the reaction chamber to a reaction temperature.

[0016] Optionally, the lithium sulfide preparation device includes a vacuum pump, which is connected to the reaction chamber and is used to extract air from the reaction chamber.

[0017] Optionally, the reactor further includes a stirrer, which extends into the reaction chamber to stir the material in the reaction chamber.

[0018] The present application also provides a method for preparing lithium sulfide, comprising the following steps:

[0019] Adding anhydrous lithium hydroxide into the reaction chamber of the reactor;

[0020] After the air in the reaction chamber is extracted, hydrogen sulfide gas is introduced through the air inlet pipe;

[0021] Raising the temperature in the reaction chamber to the reaction temperature and stirring the material in the reaction chamber;

[0022] The tail gas generated in the reaction chamber passes through the return gas pipe, the moisture detector and the gas dryer in sequence, and then re-enters the intake pipe;

[0023] When the detection values ​​obtained by the moisture detector are all lower than the threshold value within the preset detection period, the return air booster is stopped from continuing to introduce hydrogen sulfide gas, and the heating device and the stirring device are turned off;

[0024] After the reaction chamber is cooled, the hydrogen sulfide gas is discharged to obtain the lithium sulfide product.

[0025] Compared with the prior art, the beneficial effects of the present invention are:

[0026] The lithium sulfide preparation device provided in the present application includes a reactor, a return air pipe, a moisture detector and a gas dryer. The reactor has a reaction chamber, an air inlet pipe, an exhaust pipe and a discharge port; the reaction chamber is the main place where anhydrous lithium hydroxide and hydrogen sulfide gas undergo a chemical reaction. The air inlet pipe is responsible for introducing hydrogen sulfide gas into the reaction chamber, while the exhaust pipe is responsible for discharging the exhaust gas generated after the reaction is completed. At the same time, the discharge port is set at the bottom of the reaction chamber to facilitate the smooth discharge of the lithium sulfide product. In order to maximize the utilization rate of hydrogen sulfide and reduce resource waste, one end of the return air pipe is connected to the exhaust pipe, and the other end is connected to the air inlet pipe, thereby forming a recycling of the incompletely reacted hydrogen sulfide in the exhaust gas, so that the incompletely reacted hydrogen sulfide in the exhaust gas can be redirected back to the reaction chamber to continue to participate in the reaction, thereby improving the recycling rate of hydrogen sulfide. The moisture detector is located at the air inlet end of the return air pipe. The moisture detector can monitor the water content in the exhaust gas in real time. Based on the characteristic that no water is generated when the reaction between lithium hydroxide and hydrogen sulfide is complete, when the water content in the exhaust gas tends to be stable, it can be judged that the reaction has reached a complete state. In order to prevent the lithium sulfide product from undergoing a reverse reaction due to the presence of water, a gas dryer is installed at the air outlet end of the return air pipe. The exhaust gas discharged from the reaction chamber passes through the moisture detector and the gas dryer in sequence before re-entering the intake pipe. The gas dryer can effectively remove moisture from the exhaust gas and ensure that the gas reintroduced into the intake pipe is in a dry state, thereby effectively preventing the reverse reaction of lithium sulfide and further improving the purity and yield of the product.

[0027] The lithium sulfide preparation device of the present application can not only improve the utilization rate of hydrogen sulfide and reduce the treatment pressure of hydrogen sulfide during tail gas treatment, but also avoid the reverse reaction of lithium sulfide, thereby ensuring high yield and high quality of lithium sulfide products. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0029] Figure 1 It is a schematic diagram of the pipeline structure of the lithium sulfide preparation device of the present application.

[0030] Among them, the reference numerals in the figures are:

[0031] 1. Reactor; 11. Reaction chamber;

[0032] 12. Intake pipe; 13. Exhaust pipe;

[0033] 14. Discharge port; 15. Agitator;

[0034] 2. Air return pipe; 3. Moisture detector;

[0035] 4. Gas dryer; 5. Return air booster;

[0036] 6. Heater; 7. Vacuum pump. DETAILED DESCRIPTION

[0037] In order to make the technical problems, technical solutions and beneficial effects to be solved by this application more clearly understood, this application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain this application and are not intended to limit this application.

[0038] It should be noted that when an element is referred to as being “fixed on” or “disposed on” another element, it may be directly on the other element or indirectly on the other element. When an element is referred to as being “connected to” another element, it may be directly connected to the other element or indirectly connected to the other element.

[0039] It should be understood that the terms "length", "width", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on this application.

[0040] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. Throughout the description of this application, "plurality" means two or more, unless otherwise specifically defined.

[0041] Unless otherwise defined, all technical terms used hereinafter have the same meanings as those generally understood by those skilled in the art. The technical terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present invention.

[0042] like Figure 1As shown, the present application provides a lithium sulfide preparation device, including a reactor 1, a gas return pipe 2, a moisture detector 3 and a gas dryer 4.

[0043] Reactor 1 comprises a reaction chamber 11, an air inlet pipe 12, an exhaust pipe 13, and a discharge port 14. Reaction chamber 11 is the primary location for the chemical reaction between anhydrous lithium hydroxide and hydrogen sulfide gas. The air inlet pipe 12 introduces hydrogen sulfide gas into the reaction chamber 11, while the exhaust pipe 13 discharges the exhaust gas produced after the reaction. Discharge port 14 is located at the bottom of the reaction chamber 11 to facilitate the smooth discharge of the lithium sulfide product.

[0044] In order to maximize the utilization rate of hydrogen sulfide and reduce resource waste, one end of the return air pipe 2 is connected to the tail gas pipe 13, and the other end is connected to the intake pipe 12, thereby forming a recycling of the incompletely reacted hydrogen sulfide in the tail gas, so that the incompletely reacted hydrogen sulfide in the tail gas can be redirected back to the reaction chamber 11 to continue to participate in the reaction, thereby improving the recycling rate of hydrogen sulfide.

[0045] The moisture detector 3 is arranged at the air inlet end of the return air pipe 2. The moisture detector 3 can monitor the water content in the exhaust gas in real time. According to the characteristic that no water is generated when the reaction of lithium hydroxide and hydrogen sulfide is complete, when the water content in the exhaust gas tends to be stable, it can be judged that the reaction has reached a complete state.

[0046] To prevent the reverse reaction of the lithium sulfide product due to the presence of moisture, a gas dryer 4 is installed at the outlet of the return gas pipe 2. The exhaust gas discharged from the reaction chamber 11 passes through the moisture detector 3 and the gas dryer 4 before re-entering the intake pipe 12. The gas dryer 4 effectively removes moisture from the exhaust gas, ensuring that the gas re-introduced into the intake pipe 12 is dry, effectively preventing the reverse reaction of the lithium sulfide and further improving the purity and yield of the product. Desiccant agents in the gas dryer 4 include, but are not limited to, silica gel and molecular sieves.

[0047] The lithium sulfide preparation device of the present application can not only improve the utilization rate of hydrogen sulfide and reduce the treatment pressure of hydrogen sulfide during tail gas treatment, but also avoid the reverse reaction of lithium sulfide, thereby ensuring high yield and high quality of lithium sulfide products.

[0048] like Figure 1 As shown, in a specific embodiment of the present application, the lithium sulfide preparation device includes a return gas booster 5, which is arranged at the gas outlet end of the return gas pipe 2. The return gas booster 5 is used to pressurize the dried gas in the return gas pipe 2 to the same pressure as the gas in the intake pipe 12, thereby avoiding the gas backflow phenomenon that may be caused by the pressure difference.

[0049] like Figure 1As shown, in a specific embodiment of the present application, the lithium sulfide preparation apparatus includes a heater 6, which is used to heat the reaction chamber 11 to a reaction temperature. The temperature required for the reaction of lithium hydroxide and hydrogen sulfide is generally 150°C-160°C. The heater 6 includes but is not limited to a steam heater, a thermal oil heater, an electric heater, etc.

[0050] like Figure 1 As shown, in one specific embodiment of the present application, the lithium sulfide preparation apparatus includes a vacuum pump 7, which is specifically connected to a reaction chamber 11. The presence of air in the reaction chamber 11 not only interferes with the thorough mixing and contact of the reactants, but may also introduce impurities, thereby affecting the purity and quality of the final product. Therefore, the air in the reaction chamber 11 is evacuated by the vacuum pump 7 to provide a pure reaction environment for the synthesis of lithium sulfide, thereby ensuring product quality.

[0051] like Figure 1 As shown, in a specific embodiment of the present application, the reactor 1 further includes an agitator 15, which extends into the reaction chamber 11 to stir the materials in the reaction chamber 11. By properly controlling the rotational speed, the agitator 15 can ensure that the reaction materials are evenly distributed and fully contacted within the reaction chamber 11, thereby accelerating the chemical reaction process and improving the reaction efficiency. In view of the reaction characteristics of lithium hydroxide and hydrogen sulfide, the rotational speed of the agitator 15 is preferably 150 revolutions per minute (r / min), which can achieve effective mixing of the reaction materials while avoiding adverse factors such as material splashing or local overheating that may be caused by excessively high rotational speeds, thereby ensuring a smooth reaction process.

[0052] This application also provides a method for preparing lithium sulfide, comprising the following steps:

[0053] First, accurately weighed anhydrous lithium hydroxide is pre-added into the reaction chamber 11 of the reactor 1 as one of the main raw materials for the reaction.

[0054] Subsequently, the vacuum pump 7 is started to evacuate the air in the reaction chamber 11. After the vacuum operation is completed, hydrogen sulfide gas is released into the reaction chamber 11 through the air inlet pipe 12.

[0055] To ensure the full progress of the reaction, the amount of hydrogen sulfide gas introduced is not simply based on the theoretical value calculated according to the chemical reaction equation. Instead, on this basis, the reaction efficiency and gas utilization rate are comprehensively considered, and the actual supply amount is set to 1.2 to 2.0 times the theoretical value to avoid incomplete reaction due to insufficient gas.

[0056] Next, heater 6 is activated, gradually raising the temperature within reaction chamber 11 to a suitable reaction temperature range of 150°C to 160°C. This temperature range has been shown to be optimal for the reaction of lithium hydroxide and hydrogen sulfide, significantly improving the reaction rate and product purity. Simultaneously, agitator 15 is activated at a constant speed of 150 rpm to uniformly and efficiently stir the materials within reaction chamber 11, ensuring sufficient contact and mixing between the reactants.

[0057] The tail gas generated in the reaction chamber 11 mainly contains unreacted hydrogen sulfide. After passing through the return pipe 2, the tail gas passes through the moisture detector 3 and the gas dryer 4 in sequence, and then re-enters the intake pipe 12. The moisture content of the gas after passing through the gas dryer 4 must be reduced to below 5ppm.

[0058] The gas after drying passes through the return gas booster 5 to keep its pressure consistent with the gas pressure in the intake pipe 12, so that this part of the tail gas is smoothly reintroduced into the reaction chamber 11, realizing the recycling of hydrogen sulfide gas, greatly improving the utilization rate of raw materials and the economic efficiency of the reaction.

[0059] When the detection values ​​obtained by moisture detector 3 are all below a threshold value (generally less than 5 ppm) within a preset detection period (e.g., every hour), the reaction is considered to have reached its endpoint. At this point, the return air booster 5 can be stopped, the hydrogen sulfide gas supply can be cut off, and the heating and stirring devices can be turned off to allow the reaction system to cool. After the temperature in reaction chamber 11 drops to a safe operating range (below 50°C), nitrogen or other protective gas is introduced into reaction chamber 11 to displace and expel the remaining hydrogen sulfide gas. This displaced hydrogen sulfide gas can also be recycled and reused, further improving resource utilization efficiency.

[0060] Finally, when the hydrogen sulfide replacement operation is completed, the discharge port 14 is opened to obtain the lithium sulfide product.

[0061] The above description is only a preferred embodiment of the present application and is not intended to limit the present application. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present application should be included in the scope of protection of the present application.

Claims

1. A lithium sulfide preparation device, characterized in that: include: A reactor (1) having a reaction chamber (11), an air inlet pipe (12), an exhaust pipe (13) and a discharge port (14); A return air pipe (2), one end of which is connected to the tail gas pipe (13) and the other end of which is connected to the intake pipe (12); A moisture detector (3) is provided at the air inlet end of the return air pipe (2), and the moisture detector (3) is used to detect the water content of the exhaust gas in the exhaust pipe (13); A gas dryer (4) is provided at the gas outlet end of the return gas pipe (2), and the gas dryer (4) is used to dry the gas entering the gas inlet pipe (12); The tail gas discharged from the reaction chamber (11) passes through the moisture detector (3) and the gas dryer (4) in sequence, and then re-enters the air inlet pipe (12).

2. The lithium sulfide preparation device according to claim 1, characterized in that: It comprises a return air booster (5) arranged at the outlet end of the return air pipe (2), and the return air booster (5) is used to boost the pressure of the dried gas in the return air pipe (2) to the same pressure as the gas in the intake pipe (12).

3. The lithium sulfide preparation device according to claim 1, characterized in that: It comprises a heater (6), and the heater (6) is used to heat the reaction chamber (11) to a reaction temperature.

4. The lithium sulfide preparation device according to claim 1, characterized in that: It comprises a vacuum pump (7), the vacuum pump (7) being in communication with the reaction chamber (11), and the vacuum pump (7) being used to extract air from the reaction chamber (11).

5. The lithium sulfide preparation device according to claim 1, characterized in that: The reactor (1) further comprises a stirrer (15), wherein the stirrer (15) extends into the reaction chamber (11) to stir the material in the reaction chamber (11).

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