A closed system for lithium sulfide preparation device

Abstract

The utility model discloses a closed system for a lithium sulfide preparation device, which belongs to the technical field of solid-state lithium batteries and is mainly used for sealing a lithium sulfide preparation device, including a lithium sulfide preparation device and a closed unit, wherein the closed unit includes a preparation chamber filled with dry gas and sealed and an atmosphere purification module arranged in the preparation chamber; the lithium sulfide preparation device is arranged in the preparation chamber; the atmosphere purification module includes an atmosphere circulation module, the atmosphere circulation module is connected with an organic matter control module and a moisture control module, the organic matter control module is connected with a hydrogen sulfide control module, the atmosphere circulation module, the hydrogen sulfide control module, and the moisture control module are connected with the preparation chamber; the atmosphere circulation module, the organic matter control module, the hydrogen sulfide control module, and the moisture control module are electrically connected with a parameter control system. The closed system of the present application is adopted to perform secondary sealing on the lithium sulfide preparation device, so as to avoid environmental pollution caused by the generated harmful gases and materials, and ensure the quality of the prepared lithium sulfide product.

Description

Technical Field

[0001] The utility model relates to the technical field of solid-state lithium batteries, in particular to a closed system of a lithium sulfide preparation device. Background Art

[0002] Solid electrolytes will replace liquid electrolytes in lithium-based battery systems in the future due to their higher safety. Among them, sulfide electrolytes are currently the most advantageous and eye-catching electrolyte system, and lithium sulfide is an indispensable raw material for the preparation of sulfide solid electrolytes.

[0003] However, lithium sulfide is extremely sensitive to water. When exposed to the air, it easily absorbs moisture and hydrolyzes into highly toxic and flammable hydrogen sulfide gas. Therefore, the preparation of lithium sulfide must be carried out in a closed device under the protection of an inert gas. In addition, harmful gases such as hydrogen sulfide will be generated in the process of preparing lithium sulfide. Therefore, tail gas treatment equipment is usually connected to the closed lithium sulfide preparation device to treat the harmful gases before discharging them into the air. When preparing lithium sulfide, the lithium sulfide preparation device may still fail to seal. However, most of the existing lithium sulfide preparation devices focus on the chemical reaction itself, and do not involve how to avoid harmful gases and materials from leaking to the external environment to cause pollution or even damage to personnel health when the equipment used to prepare lithium sulfide fails to seal, and how to avoid external atmosphere from entering the lithium sulfide preparation device when the equipment used to prepare lithium sulfide fails to seal, resulting in a decline in product quality, potential safety hazards and impact on product quality. Utility Model Content

[0004] The technical problem to be solved by the utility model is to provide a closed system for a lithium sulfide preparation device, which is mainly used for sealing the lithium sulfide preparation device to achieve secondary sealing of the lithium sulfide preparation device, avoid environmental pollution caused by harmful gases and materials generated by the lithium sulfide preparation device, and at the same time ensure the quality of the products prepared by the lithium sulfide preparation device.

[0005] The utility model discloses a closed system of a lithium sulfide preparation device, comprising a lithium sulfide preparation device and a closed unit, wherein the closed unit comprises a preparation chamber filled with dry gas and closed, and an atmosphere purification module arranged in the preparation chamber, wherein the lithium sulfide preparation device is arranged in the preparation chamber, and the lithium sulfide preparation device is provided with an exhaust gas discharge pipe connected to the outside of the preparation chamber; the atmosphere purification module comprises an atmosphere circulation module, an organic matter control module, a hydrogen sulfide control module and a moisture control module, wherein the atmosphere circulation module is connected to the organic matter control module and the moisture control module through an air delivery pipe, wherein the organic matter control module is connected to the hydrogen sulfide control module through the air delivery pipe, wherein both the input end and the output end of the atmosphere circulation module are connected to the preparation chamber, wherein the output end of the hydrogen sulfide control module is connected to the preparation chamber and the exhaust gas discharge pipe, and wherein the output end of the moisture control module is connected to the preparation chamber and the exhaust gas discharge pipe; wherein the atmosphere circulation module, the organic matter control module, the hydrogen sulfide control module and the moisture control module are electrically connected with a parameter control system.

[0006] Furthermore, the atmosphere purification module also includes an oxygen control module, the atmosphere circulation module, the oxygen control module and the moisture control module are sequentially connected through an air pipe, and the oxygen control module is electrically connected to a parameter control system.

[0007] As a preferred embodiment, the atmosphere circulation module includes a third air pump for introducing reducing gas; the organic matter control module includes an organic matter purification column and an organic matter sensor for monitoring the organic matter content in the preparation room; the hydrogen sulfide control module includes a hydrogen sulfide purification column and a hydrogen sulfide sensor for monitoring the hydrogen sulfide content in the preparation room; the moisture control module includes a water purification column and a water sensor for monitoring the moisture content in the preparation room, and the oxygen control module includes an oxygen purification column and a first oxygen sensor for monitoring the oxygen content in the preparation room; the organic matter sensor, the hydrogen sulfide sensor, the water sensor and the first oxygen sensor are all electrically connected to the parameter control system;

[0008] A third preparation chamber air inlet valve is provided between the input end of the third air pump and the preparation chamber; a first atmosphere air inlet valve is provided between the output end of the third air pump and the input end of the organic matter purification column, and a second atmosphere air inlet valve is provided between the output end of the third air pump and the input end of the oxygen purification column; a third atmosphere air inlet valve is provided between the output end of the third air pump and the input end of the water purification column, and a total atmosphere air inlet valve is also provided between the third air pump and the first atmosphere air inlet valve, the second atmosphere air inlet valve, and the third atmosphere air inlet valve, and a third preparation chamber exhaust valve is provided between the output end of the third air pump and the preparation chamber; a second exhaust valve is provided between the output end of the hydrogen sulfide purification column and the exhaust pipe, and a fourth preparation chamber exhaust valve is provided between the output end of the hydrogen sulfide purification column and the preparation chamber; a third exhaust valve is provided between the output end of the water purification column and the exhaust pipe, and a fifth preparation chamber exhaust valve is provided between the output end of the water purification column and the preparation chamber;

[0009] The third preparation chamber air inlet valve, the third preparation chamber exhaust valve, the fourth preparation chamber exhaust valve, the fifth preparation chamber exhaust valve, the total atmosphere air inlet valve, the first atmosphere air inlet valve, the second atmosphere air inlet valve, the third atmosphere air inlet valve, the second tail gas exhaust valve and the third tail gas exhaust valve are all electrically connected to the parameter control system.

[0010] As a preferred embodiment, the organic matter purification column is provided with a first heater; the hydrogen sulfide purification column is provided with a fourth heater; the water purification column is provided with a third heater; the oxygen purification column is provided with a second heater; the first heater, the fourth heater, the third heater and the second heater are all electrically connected to the parameter control system.

[0011] Furthermore, the input end of the atmosphere circulation module is also connected to a dust filter, and the input end of the dust filter is connected to the preparation chamber.

[0012] Furthermore, an air pressure control module is provided in the preparation chamber, the input end of the air pressure control module is connected to the preparation chamber, the output end of the air pressure control module is connected to the preparation chamber and the exhaust pipe, and the air pressure control module is electrically connected to the parameter control system.

[0013] As a preferred embodiment, the air pressure control module includes a first air pump for introducing dry gas and a first air pressure sensor for monitoring the air pressure in the preparation chamber, a first preparation chamber air inlet valve is provided between the input end of the first air pump and the preparation chamber, a first preparation chamber exhaust valve is provided between the output end of the first air pump and the preparation chamber, and a first exhaust gas exhaust valve is provided between the output end of the first air pump and the exhaust pipe; the first air pressure sensor is electrically connected to the parameter control system; the first preparation chamber air inlet valve, the first preparation chamber exhaust valve and the first exhaust gas exhaust valve are all electrically connected to the parameter control system.

[0014] Furthermore, a temperature control module is provided in the preparation chamber, an input end and an output end of the temperature control module are both connected to the preparation chamber, and the temperature control module is electrically connected to the parameter control system.

[0015] As a preferred embodiment, the temperature control module includes a temperature regulator, a second air pump and a temperature sensor for monitoring the temperature in the preparation chamber, the input end of the second air pump is connected to the preparation chamber, the output end of the second air pump is connected to the input end of the temperature regulator, and the output end of the temperature regulator is connected to the preparation chamber; a second preparation chamber air inlet valve is provided between the input end of the second air pump and the preparation chamber, and a second preparation chamber exhaust valve is provided between the output end of the temperature regulator and the preparation chamber; the temperature regulator and the temperature sensor are electrically connected to the parameter control system; the second preparation chamber air inlet valve and the second preparation chamber exhaust valve are both electrically connected to the parameter control system.

[0016] Furthermore, a transition chamber connected to the preparation chamber is provided on one side of the preparation chamber, and the transition chamber is filled with dry gas.

[0017] Furthermore, it also includes a tail gas treatment unit for treating exhaust gas from the preparation room and the lithium sulfide preparation device. The tail gas treatment unit is arranged outside the preparation room. The tail gas treatment unit includes an absorption device, and the absorption device is connected to the tail gas emission pipe.

[0018] As a preferred embodiment, the absorption equipment includes a sedimentation tank, a packing absorption tank, a spray tower and an absorption liquid tank which are connected in sequence, the air inlet of the sedimentation tank is connected to the exhaust gas emission pipe, the air outlet of the sedimentation tank is connected to the air inlet of the packing absorption tank, the air outlet of the packing absorption box is connected to the air inlet of the spray tower body, the lower part of the spray tower body is connected to the absorption liquid tank, and the air outlet of the spray tower is connected to the external environment.

[0019] As a preferred embodiment, the exhaust gas treatment unit also includes an induced draft device, which includes an induced draft fan and an exhaust chimney, the air inlet of the induced draft fan is connected to the air outlet of the spray tower; the exhaust chimney is vertically arranged at the air outlet of the induced draft fan, and the air outlet of the exhaust chimney is higher than the air outlet of the induced draft fan.

[0020] As a preferred embodiment, a pH sensor for monitoring the pH value in the absorption liquid tank is provided in the absorption liquid tank, a flow meter for monitoring the gas flow rate is provided on the induced draft fan, and the pH sensor and the flow meter are electrically connected to the parameter control system.

[0021] Furthermore, it also includes a gas control unit, which is arranged outside the preparation room. The gas control unit includes a dry air storage tank, an inert gas storage tank and a reducing gas storage tank. The output end of the dry air storage tank is connected to the preparation room, the output end of the inert gas storage tank is connected to the preparation room and the lithium sulfide preparation device, the output end of the reducing gas storage tank is connected to the input end of the atmosphere circulation module, and the dry air storage tank, the inert gas storage tank and the reducing gas storage tank are electrically connected to the parameter control system.

[0022] As a preferred embodiment, a fourth air pump is provided at the input end of the dry air storage tank, a dehumidification device is provided at the input end of the fourth air pump, the input end of the dehumidification device is connected to the air, an air intake valve is provided at the input end of the dehumidification device, and the air intake valve is electrically connected to the parameter control system.

[0023] As a preferred embodiment, a monitoring meter for monitoring the pressure and flow rate of the inert gas is further provided between the inert gas storage tank and the lithium sulfide preparation device, and the monitoring meter is electrically connected to the parameter control system.

[0024] The beneficial effects of the utility model are:

[0025] 1. By placing the lithium sulfide preparation device in a closed preparation room, even if the lithium sulfide preparation device leaks, the leaked harmful gases or materials will remain in the preparation room, and will not cause environmental pollution; at the same time, dry gas is input into the preparation room, so that even if the lithium sulfide preparation device leaks, the dry gas in the preparation room will enter the lithium sulfide preparation device without affecting the quality of the product, thereby effectively ensuring the operational safety and product quality in the lithium sulfide preparation process.

[0026] 2. By setting up a moisture control module, an organic matter control module, and a hydrogen sulfide control module, the water, organic matter, hydrogen sulfide, etc. in the atmosphere inside the preparation room are monitored in real time, and transmitted to the parameter control system during the preparation of lithium sulfide. The parameter control system determines and controls the start and stop of the atmosphere circulation module, the organic matter control module, the hydrogen sulfide control module or the moisture control module, and absorbs and purifies the organic matter, hydrogen sulfide, water, etc. in the atmosphere in the preparation room. The process gas leaked during the feeding, reaction process, and material extraction of the lithium sulfide preparation device can be quickly absorbed and purified and then discharged to the external environment, thereby achieving the purpose of environmental protection and protecting the health of operators.

[0027] 3. By connecting the output ends of the atmosphere circulation module and the hydrogen sulfide control module and the moisture control module with the preparation room, the atmosphere in the preparation room can continue to be discharged into the preparation room after being purified by the organic matter control module, the hydrogen sulfide control module or the moisture control module, so that the atmosphere in the preparation room continues to circulate, greatly reducing the amount of dry air required to be input into the preparation room, thereby reducing the cost of preparing lithium sulfide. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 : A schematic diagram of the connection of each unit of a closed system of a lithium sulfide preparation device;

[0029] Figure 2 : Schematic diagram of gas control unit;

[0030] Figure 3 : Schematic diagram of closed unit;

[0031] Figure 4 : Schematic diagram of the second closed unit;

[0032] Figure 5 : Schematic diagram of exhaust gas treatment unit;

[0033] Figure 6 : Schematic diagram of the second exhaust gas treatment unit;

[0034] Figure 7 : Schematic diagram of the connection between the spray tower and the absorption liquid tank.

[0035] Figure numerals: 1-lithium sulfide preparation device; 11-first inert gas inlet valve; 111-monitoring meter; 12-exhaust valve of tail gas of preparation device; 2-parameter control system; 3-gas control unit; 31-dry air storage tank; 311-fourth air pump; 312-dehumidification equipment; 313-air inlet valve; 32-inert gas storage tank; 33-reducing gas storage tank; 4-sealed unit; 41-preparation chamber; 42-air pressure control module; 421-first air pressure sensor; 422-first air pump; 423-first working gas inlet valve; 424-second working gas inlet valve; 42 5-first preparation chamber air inlet valve; 426-first preparation chamber exhaust valve; 427-first tail gas exhaust valve; 43-temperature control module; 431-temperature sensor; 432-second air pump; 433-temperature regulator; 434-second preparation chamber air inlet valve; 435-second preparation chamber exhaust valve; 44-atmosphere circulation module; 441-third air pump; 442-dust filter; 443-reducing gas air inlet valve; 444-third preparation chamber air inlet valve; 445-third preparation chamber exhaust valve; 446-total atmosphere air inlet valve; 45-organic matter control module; 451-organic matter sensor ; 452-organic purification column; 453-first heater; 454-first atmosphere intake valve; 46-oxygen control module; 461-first oxygen sensor; 462-oxygen purification column; 463-second heater; 464-second atmosphere intake valve; 47-moisture control module; 471-water sensor; 472-water purification column; 473-third heater; 474-third atmosphere intake valve; 475-fifth preparation room exhaust valve; 476-third tail gas exhaust valve; 48-hydrogen sulfide control module; 481-hydrogen sulfide sensor; 482-hydrogen sulfide purification column; 483-first Four heaters; 484-the fourth preparation room exhaust valve; 485-the second tail gas exhaust valve; 49-the transition chamber; 491-the second inert gas inlet valve; 492-the dry air inlet valve; 493-the transition chamber exhaust valve; 494-the second oxygen sensor; 5-the tail gas treatment unit; 51-the absorption equipment; 511-the sedimentation box; 512-the packing absorption box; 513-the spray tower; 5131-the spray pump; 5132-the porous partition; 514-the absorption liquid tank; 5141-the pH sensor; 52-the induced draft equipment; 521-the induced draft fan; 5211-the flow meter; 522-the exhaust pipe. DETAILED DESCRIPTION

[0036] The utility model is further described below.

[0037] The utility model provides a closed system for a lithium sulfide preparation device, which is mainly used for the closed system of a hydrogen sulfide preparation device, such as Figure 1-Figure 4As shown, it includes a lithium sulfide preparation device 1, and also includes a closed unit 4, the closed unit 4 includes a preparation chamber 41 filled with dry gas and closed, and an atmosphere purification module arranged in the preparation chamber 41, the lithium sulfide preparation device 1 is arranged in the preparation chamber 41, and the lithium sulfide preparation device 1 is provided with an exhaust gas discharge pipe connected to the outside of the preparation chamber 41; the atmosphere purification module includes an atmosphere circulation module 44, an organic matter control module 45, a hydrogen sulfide control module 48 and a moisture control module 47, the atmosphere circulation module 44 is connected to the organic matter control module 45 through a gas transmission pipe , the moisture control module 47 is connected, the organic matter control module 45 is connected to the hydrogen sulfide control module 48 through the gas pipe, the input end and the output end of the atmosphere circulation module 44 are both connected to the preparation chamber 41, the output end of the hydrogen sulfide control module 48 is connected to the preparation chamber 41 and the exhaust gas emission pipe, and the output end of the moisture control module 47 is connected to the preparation chamber 41 and the exhaust gas emission pipe; the atmosphere circulation module 44, the organic matter control module 45, the hydrogen sulfide control module 48 and the moisture control module 47 are electrically connected to the parameter control system 2.

[0038] The closed unit 4 includes a closed preparation chamber 41 and an organic matter control module 45, a hydrogen sulfide control module 48, and a moisture control module 47 arranged in the preparation chamber 41; the preparation chamber 41 can be composed of one or more materials selected from the group consisting of walls, glass, metal, and organic panels with good airtightness and acid and alkali corrosion resistance. A lithium sulfide preparation device 1 is placed in the preparation chamber 41, and the lithium sulfide preparation device 1 is provided with a tail gas emission pipe for discharging waste gas generated by the lithium sulfide preparation device 1 during the lithium sulfide preparation process out of the preparation chamber 41. It should be noted that the gas discharged from the tail gas emission pipe of the lithium sulfide preparation device 1 is gas treated by the lithium sulfide preparation device 1. The closed preparation chamber 41 is filled with dry gas to prevent the original atmosphere in the preparation chamber 41 from entering the lithium sulfide preparation device and affecting the quality of the prepared lithium sulfide when the lithium sulfide preparation device 1 fails to seal and leaks. The dry gas can be dry air or inert gas. Such gas does not contain water and will not react with lithium sulfide, hydrogen sulfide, etc., and will not affect the normal preparation of lithium sulfide, thereby ensuring the quality of lithium sulfide products. An atmosphere purification module is provided in the preparation chamber 41 to purify the harmful gases or substances leaked from the lithium sulfide preparation device 1. Specifically, the atmosphere purification module includes an atmosphere circulation module 44, an organic matter control module 45, and a hydrogen sulfide control module 48. The atmosphere in the preparation chamber 41 is guided to enter the organic matter control module 45 in sequence through the atmosphere circulation module 44, and the content of organic matter and hydrogen sulfide contained in the atmosphere of the preparation chamber 41 is monitored and adsorbed to prevent harmful gases or substances from being directly discharged from the preparation chamber 41 and causing environmental pollution, thereby achieving environmental protection and protecting operators. For the purpose of health of employees, the hydrogen sulfide control module 48 is connected to the back of the organic matter control module 45, and the organic matter in the gas is first processed by the organic matter control module 45 to prevent the gas containing organic matter from entering the hydrogen sulfide control module 48 for reaction; the atmosphere purification module also includes a moisture control module 47, and the moisture in the preparation chamber 41 is adsorbed by the moisture control module 47, so that the atmosphere in the preparation chamber 41 is always kept dry, and the atmosphere in the preparation chamber 41 is prevented from entering the lithium sulfide preparation device 1 and affecting the quality of the lithium sulfide product; at the same time, the output ends of the atmosphere circulation module 44, the hydrogen sulfide control module 48, and the moisture control module 47 are connected to the preparation chamber 41, so that the atmosphere in the preparation chamber 41 can continue to be discharged into the preparation chamber 41 after being purified by the organic matter control module 45, the hydrogen sulfide control module 48 or the moisture control module 47, so that the atmosphere in the preparation chamber 41 continues to circulate, greatly reducing the amount of dry air required to be input into the preparation chamber 41, thereby reducing the cost of preparing lithium sulfide.The above-mentioned organic matter control module 45, hydrogen sulfide control module 48, and moisture control module 47 can all adopt existing organic matter adsorption systems, hydrogen sulfide purification systems, and moisture adsorption systems; at the same time, the preparation room 41 is also provided with corresponding observation windows and sealed doors. The observation window is used to observe the situation in the preparation room 41 and whether each module is working normally. The sealed door is used for personnel to enter and exit, put raw materials into the lithium sulfide preparation device 1, and inspect each module in the preparation room 41.

[0039] In summary, by placing the lithium sulfide preparation device 1 in a closed preparation chamber 41, even if the lithium sulfide preparation device 1 leaks, the leaked harmful gases or materials will remain in the preparation chamber 41, and will not cause environmental pollution; at the same time, dry gas is input into the preparation chamber 41, so that even if the lithium sulfide preparation device 1 leaks, the dry gas in the preparation chamber 41 will not affect the quality of the product even if it enters the lithium sulfide preparation device 1, thereby effectively ensuring the operational safety and product quality in the lithium sulfide preparation process; by setting a moisture control module 47, an organic matter control module 45, and a hydrogen sulfide control module 48, the water, organic matter, hydrogen sulfide, etc. in the internal atmosphere of the preparation chamber 41 are monitored in real time, and transmitted to the parameter control system 2 during the lithium sulfide preparation period, and the parameter control system 2 determines and controls the atmosphere circulation module 44, the organic matter control module 45, and the hydrogen sulfide control module 48. The start and stop of the control module 45, the hydrogen sulfide control module 48 or the moisture control module 47 absorbs and purifies the organic matter, hydrogen sulfide, water, etc. in the atmosphere of the preparation chamber 41, and can quickly absorb and purify the process gas leaked during the feeding, reaction process and material collection of the lithium sulfide preparation device 41 and discharge it into the external environment, so as to achieve the purpose of environmental protection and protecting the health of operators; by connecting the atmosphere circulation module 44 and the output ends of the hydrogen sulfide control module 48 and the moisture control module 47 with the preparation chamber 41, the atmosphere in the preparation chamber 41 can continue to be discharged into the preparation chamber 41 after being purified by the organic matter control module 45, the hydrogen sulfide control module 48 or the moisture control module 47, so that the atmosphere in the preparation chamber 41 continues to circulate, which greatly reduces the amount of dry air required to be input into the preparation chamber 41, thereby reducing the cost of preparing lithium sulfide.

[0040] When an inert gas is used as the drying gas inside the preparation chamber 41, the oxygen content in the preparation chamber 41 needs to be controlled to ensure the safety of the operators when entering and leaving the preparation chamber 41. The atmosphere purification module also includes an oxygen control module 46. The atmosphere circulation module 44, the oxygen control module 46 and the moisture control module 47 are sequentially connected through a gas pipeline. The oxygen control module 46 is electrically connected to the parameter control system 2. The oxygen content in the preparation chamber 41 is monitored and oxygen adsorption is processed by the oxygen control module 46 to control the oxygen content in the preparation chamber 41. Then, the oxygen control module 46 controls the oxygen content in the preparation chamber 41. 46 is connected to the input end of the moisture control module 47 to prevent the water generated by the oxygen control module 46 when adsorbing and treating oxygen from re-entering the preparation chamber 41 and affecting the quality of the lithium sulfide product; when dry air is used as the drying gas in the preparation chamber 41, in order to prevent the oxygen adsorbing material in the oxygen control module 46 from being saturated and failing when the dry air passes through the oxygen control module 46, the oxygen control module 46 needs to be closed. At this time, the input end of the moisture purification module 47 is connected to the output end of the atmosphere circulation module 44, so that the gas input by the atmosphere circulation module 44 bypasses the oxygen control module 46 and directly enters the water purification column 472.

[0041] Specifically, the atmosphere circulation module 44 includes a third air pump 441 for introducing reducing gas; the organic matter control module 45 includes an organic matter purification column 452 and an organic matter sensor 451 for monitoring the organic matter content in the preparation chamber 41; the hydrogen sulfide control module 48 includes a hydrogen sulfide purification column 482 and a hydrogen sulfide sensor 481 for monitoring the hydrogen sulfide content in the preparation chamber 41; the moisture control module 47 includes a water purification column 472 and a water sensor 471 for monitoring the moisture content in the preparation chamber 41, and the oxygen control module 46 includes an oxygen purification column 462 and a water sensor 461 for monitoring A first oxygen sensor 461 for measuring the oxygen content in the preparation chamber 41; the organic matter sensor 451, the hydrogen sulfide sensor 481, the water sensor 471 and the first oxygen sensor 461 are all electrically connected to the parameter control system 2; a third preparation chamber air intake valve 444 is provided between the input end of the third air pump 441 and the preparation chamber 41; a first atmosphere air intake valve 454 is provided between the output end of the third air pump 441 and the input end of the organic matter purification column 452, and a second atmosphere air intake valve 464 is provided between the output end of the third air pump 441 and the input end of the oxygen purification column 462; A third atmosphere inlet valve 474 is provided between the output end of the third air pump 441 and the input end of the water purification column 472, and a total atmosphere inlet valve 446 is provided between the third air pump 441 and the first atmosphere inlet valve 454, the second atmosphere inlet valve 464, and the third atmosphere inlet valve 474. A third preparation chamber exhaust valve 445 is provided between the output end of the third air pump 441 and the preparation chamber 41; a second exhaust gas exhaust valve 485 is provided between the output end of the hydrogen sulfide purification column 482 and the exhaust pipe, and a fourth preparation chamber exhaust valve 446 is provided between the output end of the hydrogen sulfide purification column 482 and the preparation chamber 41. Valve 484; a third exhaust gas exhaust valve 476 is provided between the output end of the water purification column 472 and the exhaust pipe, and a fifth preparation chamber exhaust valve 475 is provided between the output end of the water purification column 472 and the preparation chamber 41; the third preparation chamber air inlet valve 444, the third preparation chamber exhaust valve 445, the fourth preparation chamber exhaust valve 484, the fifth preparation chamber exhaust valve 475, the total atmosphere air inlet valve 446, the first atmosphere air inlet valve 454, the second atmosphere air inlet valve 464, the third atmosphere air inlet valve 474, the second exhaust gas exhaust valve 485 and the third exhaust gas exhaust valve 476 are all electrically connected to the parameter control system.

[0042] The atmosphere circulation module 44 includes a third air pump 441 that can pass reducing gas and is arranged in the preparation chamber 41. In order to circulate the gas in the preparation chamber 41 and enable the gas discharged through the air pressure control module 42 and the temperature control module 43 to circulate in the preparation chamber 41, the input end of the third air pump 441 is connected to the preparation chamber 41, and the output end of the third air pump 441 is connected to the preparation chamber 41, and is controlled by the third preparation chamber air inlet valve 444 and the third preparation chamber exhaust valve 445; in order to purify the gas in the preparation chamber 41 when the lithium sulfide preparation device 1 leaks and harmful gas enters the preparation chamber 41, the output end of the third air pump 441 is connected to the input end of the organic purification column 452, the oxygen purification column 453 and the oxygen purification column 454. The input end of the chemical column 462 and the input end of the water purification column 472 are connected, and the third air pump 441 is controlled by the first atmosphere air inlet valve 454, the second atmosphere air inlet valve 464, and the third atmosphere air inlet valve 474 to transport the reducing gas to the corresponding position; and the third air pump 441 is controlled by the total atmosphere air inlet valve 446 to be used for circulating the atmosphere in the preparation chamber 41 or for transporting reducing gas to purify the gas in the preparation chamber 41; when the third air pump 441 is used to transport reducing gas to purify the gas in the preparation chamber 41, the third preparation chamber air inlet valve 444 and the total atmosphere air inlet valve 446 are opened, and the first atmosphere air inlet valve 454, the second atmosphere air inlet valve 464 or the third atmosphere air inlet valve 474 are opened as needed, and the third preparation chamber exhaust valve 445 is closed.The output end of the hydrogen sulfide purification column 482 is connected to the input end of the preparation chamber 41 and the absorption device 51, and the second tail gas exhaust valve 485 and the fourth preparation chamber exhaust valve 484 control the discharge path of the gas through the organic control module 45 and the hydrogen sulfide control module 48; the output end of the water purification column 472 is connected to the input end of the preparation chamber 41 and the absorption device 51, and the third tail gas exhaust valve 476 and the fifth preparation chamber exhaust valve 475 control the discharge path of the gas through the oxygen control module 46 and the moisture control module 47; when the organic matter sensor 451 detects that the organic matter in the preparation chamber 41 is higher than the warning value or the organic matter reduction rate is low and is fed back to the parameter control system 2, or the hydrogen sulfide sensor When the sensor 481 detects that the hydrogen sulfide in the preparation chamber 41 is higher than the warning value or the rate of hydrogen sulfide reduction is low and feeds back to the parameter control system 2, the total atmosphere intake valve 446 and the first atmosphere intake valve 454 are opened, the fourth preparation chamber exhaust valve 484 is closed and the second tail gas exhaust valve 485 is opened, and then the organic matter purification column 452 and the hydrogen sulfide purification column 482 are used to reduce the organic matter content and hydrogen sulfide content in the preparation chamber 41; when the first oxygen sensor 461 detects that the oxygen content in the preparation chamber 41 is higher than the warning value or the rate of oxygen content reduction is low and feeds back to the parameter control system 2, or the water sensor 471 detects that the moisture content in the preparation chamber 41 is higher than the warning value or the rate of moisture content reduction is low and feeds back When the parameter control system 2 is reached, the total atmosphere air intake valve 446, the second atmosphere air intake valve 465, and the third atmosphere air intake valve 474 are opened, the fifth preparation chamber exhaust valve 475 is closed, and the third tail gas exhaust valve 476 is opened, and then the water purification column 472 and the oxygen purification column 462 are used to reduce the moisture content and oxygen content in the preparation chamber 41; the moisture control module 47 is arranged after the oxygen control module 46 to ensure that whether inert gas or dry air is used as the working gas in the preparation chamber 41, that is, whether the oxygen control module 46 is closed or not, it will not affect the gas treated by the oxygen purification column 462 or the water purification column 472 to be discharged into or out of the preparation chamber 41, and at the same time The oxygen purification column 462 generates water after a reduction reaction with hydrogen at high temperature, which can then be treated by the water purification column 472; when it is necessary to replace the organic purification column 452 or the hydrogen sulfide purification column 482, close the first atmosphere intake valve 454, the fourth preparation chamber exhaust valve 484, and the second tail gas exhaust valve 485; when it is necessary to replace the oxygen purification column 462 or the water purification column 472, close the second atmosphere intake valve 464, the third atmosphere intake valve 474, the third tail gas exhaust valve 476, and the fifth preparation chamber exhaust valve 475; the above-mentioned organic purification column can use activated carbon, the hydrogen sulfide purification column can use a complex desulfurization catalyst or a molecular sieve, the oxygen purification column can use a copper catalyst, and the water purification column can use a molecular sieve.

[0043] It should be noted that during the lithium sulfide preparation process, the organic matter control module 45 and the hydrogen sulfide control module 48 are generally open, so that the atmosphere circulation module 44 continuously transports the internal gas of the preparation chamber 41 through the organic matter purification column 452 through the third air pump 441 to reduce the organic matter in the atmosphere of the preparation chamber 41, and the internal gas of the preparation chamber 41 continuously passes through the hydrogen sulfide purification column 482 through the organic matter control module 45 to reduce the hydrogen sulfide in the atmosphere of the preparation chamber 41; the moisture control module 47 is generally open, so that the atmosphere circulation module 44 continuously transports the internal gas of the preparation chamber 41 through the third air pump 441 to pass through the water purification column 472 to reduce the moisture in the atmosphere of the preparation chamber 41, so as to avoid leakage in the lithium sulfide preparation device 1. After the atmosphere in the preparation chamber 41 enters the lithium sulfide preparation device 1, the water in the atmosphere reacts with lithium sulfide, thereby reducing the quality of the lithium sulfide product. At the same time, when dry air is used as the working gas in the preparation chamber 41, due to the high oxygen content in the dry gas, in order to avoid the dry gas passing through the oxygen control module 46 and causing the oxygen purification column 462 to be saturated and fail, the oxygen control module 46 needs to be closed. At this time, the input end of the water purification column 472 is connected to the output end of the third air pump 441, and the gas input by the atmosphere circulation module 44 is controlled by the third atmosphere inlet valve 474 to bypass the oxygen control module 46 and directly enter the water purification column 472.

[0044] In order to reduce the replacement frequency of the organic purification column 452, the hydrogen sulfide purification column 482, the water purification column 472, and the oxygen purification column 462 and reduce the use cost of the closed system, the organic purification column 452 is provided with a first heater 453; the hydrogen sulfide purification column 482 is provided with a fourth heater 483; the water purification column 472 is provided with a third heater 473; the oxygen purification column 462 is provided with a second heater 463; the first heater 453, the fourth heater 483, the third heater 473, the second heater 463 are all electrically connected to the parameter control system 2; when the atmosphere circulation module 44 is fed with reducing gas, the corresponding organic purification column 452, hydrogen sulfide purification column 482, water purification column 472, and oxygen purification column 462 are heated by the additional first heater 453, fourth heater 483, third heater 473, and second heater 463, and the organic matter adsorbed by the organic purification column 452 is desorbed at high temperature and taken away by the mixed gas; the hydrogen sulfide adsorbed by the hydrogen sulfide purification column 482 is desorbed at high temperature and taken away by the mixed gas, and the oxygen purification column 46 2 is reduced by the reducing gas under heating, and the generated water is taken away by the mixed gas. At this time, the fourth preparation chamber exhaust valve 484 and the fifth preparation chamber exhaust valve 475 need to be closed, and the second tail gas exhaust valve 485 and the third tail gas exhaust valve 476 need to be opened to discharge the gas obtained after being heated by the first heater 453, the fourth heater 483, the third heater 473, and the second heater 463. The water adsorbed by the water purification column 472 is desorbed at high temperature and taken away by the mixed gas; when the organic matter purification column 452, the hydrogen sulfide purification column 482, the water purification column 473, the water purification column 474, the water purification column 476 ... After the column 472 and the oxygen purification column 462 have been working for a period of time, the corresponding first heater 453, the fourth heater 483, the third heater 473, and the second heater 463 can be turned on through the parameter control system 2 to process the substances attached thereto, so that the organic purification column 452, the hydrogen sulfide purification column 482, the water purification column 472, and the oxygen purification column 462 can continue to work, thereby reducing the replacement frequency of the organic purification column 452, the hydrogen sulfide purification column 482, the water purification column 472, and the oxygen purification column 462, and reducing the use cost of the closed system.

[0045] In order to prevent the dust generated during the lithium sulfide preparation process from escaping from the lithium sulfide preparation device 1 and entering the organic purification column 452, the hydrogen sulfide purification column 482, the oxygen purification column 462 or the water purification column 472 through the atmosphere circulation module 44, thereby affecting their normal operation; the input end of the atmosphere circulation module 44 is also connected to a dust filter 442, and the input end of the dust filter 442 is connected to the preparation chamber 41; specifically, the output end of the dust filter 442 is connected to the input end of the third air pump 441 of the atmosphere circulation module 44, and the dust filter 442 is used to filter out the dust in the gas entering the third air pump 441 in advance, thereby effectively filtering out the dust entering the organic control module 45, the oxygen control module 46, the moisture control module 47, and the dust content that re-enters the preparation chamber 41 after circulation.

[0046] To ensure that the preparation chamber 41 is filled with dry gas, and that the air pressure in the preparation chamber 41 is not too high when the lithium sulfide preparation device 2 leaks, and the normal working air pressure in the preparation chamber 41 is maintained, the preparation chamber 41 is also provided with an air pressure control module 42, the input end of the air pressure control module 42 is connected to the preparation chamber 41, the output end of the air pressure control module 42 is connected to the preparation chamber 41 and the exhaust pipe, and the air pressure control module 42 is electrically connected to the parameter control system 2; the air pressure control module 42 is set to monitor the air pressure in the preparation chamber 41 in real time The range of the preparation chamber 41 is to ensure the normal use of the lithium sulfide preparation device and to prevent the excessive air pressure in the preparation chamber 41 from entering the lithium sulfide preparation device and affecting the quality of the lithium sulfide product. As a preferred method, the dry gas can be filled in and the internal gas of the preparation chamber 41 can be discharged to ensure that the air pressure in the preparation chamber 41 is maintained within the normal working range. The air pressure control module 42 includes a first air pump 422 for introducing dry gas and a first air pressure sensor 421 for monitoring the air pressure in the preparation chamber 41. A first air pressure sensor 421 is provided between the input end of the first air pump 442 and the preparation chamber 41. The first preparation chamber air inlet valve 425, the first preparation chamber exhaust valve 426 is provided between the output end of the first air pump 422 and the preparation chamber 41, and the first exhaust gas exhaust valve 427 is provided between the output end of the first air pump 422 and the exhaust gas exhaust pipe; the first air pressure sensor 421 is electrically connected to the parameter control system 2; the first preparation chamber air inlet valve 425, the first preparation chamber exhaust valve 426, and the first exhaust gas exhaust valve 427 are all electrically connected to the parameter control system 2; when the first air pressure sensor 421 monitors that the pressure in the preparation chamber 41 is higher than the set pressure range After the first air pump 422 is surrounded and fed back to the parameter control system 2, the first air pump 422 starts working, and the first preparation chamber air inlet valve 425 and the first tail gas exhaust valve 427 are opened to discharge the gas inside the preparation chamber 41; when the first air pressure sensor 421 detects that the pressure in the preparation chamber 41 is lower than the set pressure range and feeds back to the parameter control system 2, the first air pump 422 starts working, and at the same time the first preparation chamber exhaust valve 426 is opened, the first air pump 422 is used to input dry gas into the preparation chamber 41, thereby ensuring that the air pressure in the preparation chamber 41 is within the normal working range.

[0047] In order to keep the temperature in the preparation chamber 41 at a temperature suitable for preparing lithium sulfide, a temperature control module 43 is also provided in the preparation chamber 41. The input and output ends of the temperature control module 43 are both connected to the preparation chamber 41, and the temperature control module 43 is electrically connected to the parameter control system 2; the temperature in the preparation chamber 41 is monitored in real time by the temperature control module 43 and the temperature in the preparation chamber 41 is regulated. Specifically, a temperature control system similar to that used in an existing greenhouse can be used. As a preferred embodiment, the temperature control module 43 used in the closed system of the lithium sulfide preparation device includes a temperature regulator 433, a second air pump 432 and a temperature controller 433 for monitoring the temperature in the preparation chamber 41. sensor 431, the input end of the second air pump 432 is connected to the preparation chamber 41, the output end of the second air pump 432 is connected to the input end of the temperature regulator 433, and the output end of the temperature regulator 433 is connected to the preparation chamber 41; a second preparation chamber air inlet valve 434 is provided between the input end of the second air pump 432 and the preparation chamber 41, and a second preparation chamber exhaust valve 435 is provided between the output end of the temperature regulator 433 and the preparation chamber 41; the temperature regulator 433, the second air pump 432, and the temperature sensor 431 are electrically connected to the parameter control system 2; the second preparation chamber air inlet valve 434 and the second preparation chamber exhaust valve 435 are both electrically connected to the parameter control system 2. When the temperature sensor 431 detects that the temperature in the preparation chamber 41 exceeds the set temperature range and feeds back to the parameter control system 2, the parameter control system 2 controls the second air pump 432 and the temperature regulator 433 to start working, and opens the second preparation chamber air inlet valve 434 and the second preparation chamber exhaust valve 435. The gas in the preparation chamber 41 is cooled or heated through the heat exchange component of the temperature regulator 433 via the second air pump 432 until the temperature in the preparation chamber 41 reaches the set temperature range.

[0048] In order to prevent operators from bringing external water-containing air into the preparation chamber 41 when entering and exiting the preparation chamber 41 to add raw materials required for lithium sulfide preparation or to inspect and replace the organic control module 45, the hydrogen sulfide control module 48, the moisture control module 47, and the oxygen control module 46, resulting in a decrease in the quality of the product produced by the lithium sulfide preparation device 1; a transition chamber 49 connected to the preparation chamber 41 is also provided on one side of the preparation chamber 41, and the transition chamber 49 is filled with dry gas; by setting up the transition chamber 49 connected to the preparation chamber 41, it is possible to effectively avoid direct entry and exit of the preparation chamber 41, resulting in external gas entering the preparation chamber 41 and affecting the normal preparation of lithium sulfide, and at the same time, it is also possible to avoid the gas in the preparation chamber 41 escaping to the external environment and affecting the external environment. The dry gas can be dry gas or inert gas, and it should be noted that the dry gas used in the transition chamber 49 and the preparation chamber 41 should be consistent. When the operator needs to put materials into the preparation chamber 41, and the preparation chamber 41 and the transition chamber 49 are filled with inert gas, before the operator enters the preparation chamber 41, dry air is used to replace the atmosphere in the preparation chamber 41 and the transition chamber 49. In order to facilitate monitoring of the oxygen content in the preparation chamber 41 and the transition chamber 49 to reach an oxygen content value that is safe for people to enter and exit, a first oxygen sensor 461 is set in the preparation chamber 41, and a second oxygen sensor 494 is set in the transition chamber 49 to ensure the safe entry and exit of the operator. Under conditions known to those skilled in the art, an air inlet for inputting dry gas and an air outlet for exhausting gas in the transition chamber 49 can be set on the transition chamber 49.

[0049] In order to enhance the purification effect of the exhaust gas discharged from the preparation chamber 41 and the lithium sulfide preparation device 1 and ensure that the exhaust gas does not affect the external environment, the closed system of the lithium sulfide preparation device also includes an exhaust gas treatment unit 5 for treating the exhaust gas from the preparation chamber 41 and the lithium sulfide preparation device 1, wherein the exhaust gas treatment unit 5 is arranged outside the preparation chamber 41, and the exhaust gas treatment unit 5 includes an absorption device 51, and the absorption device 51 is connected to the exhaust gas emission pipe; by providing the exhaust gas treatment unit 5 connected to the exhaust gas emission pipe, the exhaust gas treated by the lithium sulfide preparation device 1 and the exhaust gas treated by the atmosphere purification module arranged in the preparation chamber 41 can be treated again after being discharged, especially the exhaust gas treatment of the gas brought out when the adsorbents in the organic matter control module 45, the hydrogen sulfide control module 48, the oxygen control module 46 and the moisture control module 47 are reduced and cleaned by the reducing gas, so as to avoid the harmful gases or substances therein being directly discharged into the air and polluting the environment. The absorption device 51 can adopt an existing spray tower or alkaline solution absorption box for treating hydrogen sulfide. The gas discharged from the preparation chamber 41 is input into the absorption device 51, and the harmful gas and dust therein are removed by the reaction of the gas and the alkaline solution to achieve clean exhaust gas discharge, thereby preventing the harmful gas or dust generated during the lithium sulfide preparation process from polluting the external environment.

[0050] In order to enhance the purification effect of the exhaust gas discharged from the preparation chamber 41 and the lithium sulfide preparation device 1 and ensure that the exhaust gas does not affect the external environment, the absorption equipment 51 includes a sedimentation tank 511, a packing absorption tank 512, a spray tower 513 and an absorption liquid tank 514 which are connected in sequence, the air inlet of the sedimentation tank 511 is connected to the exhaust gas discharge pipe, the air outlet of the sedimentation tank 511 is connected to the air inlet of the packing absorption tank 512, the air outlet of the packing absorption box 512 is connected to the air inlet of the spray tower 513, the lower part of the spray tower 513 is connected to the absorption liquid tank 514, and the air outlet of the spray tower 513 is connected to the external environment.

[0051] By setting the settling box 511, the solid particles in the collected tail gas can be intercepted to achieve the purpose of settling the tail gas; the setting of the packing absorption box 512 can adsorb the collected tail gas and absorb the organic matter, part of the acidic substances and hydrogen sulfide in the tail gas; by setting the spray tower 513 and the absorption liquid tank 514, the residual acidic substances and hydrogen sulfide in the tail gas after adsorption are removed, and then the purified gas is discharged into the air, and the harmful gases and dust therein are removed through settling, packing absorption and spraying alkali liquid droplet absorption, further reducing the emission concentration of hydrogen sulfide, and the clean tail gas is emptied. In order to ensure the tail gas treatment effect, the air inlets of the settling box 511, the packing absorption box 512 and the spray tower 513 are all located below the equipment, and the air outlets of the settling box 511, the packing absorption box 512 and the spray tower 513 are all located above the equipment, so that the tail gas can be better treated from bottom to top when entering the corresponding equipment.

[0052] The above-mentioned sedimentation tank 511, filler absorption box 512, spray tower 513 and absorption liquid tank 514 can all adopt the structure of the prior art. Specifically, a plurality of interlaced perforated baffles can be arranged in the sedimentation tank 511 to intercept solid particles and realize the sedimentation of tail gas; the filler absorption box 512 is tightly filled with activated carbon, and the tail gas passing through the sedimentation tank 511 enters from the bottom of the filler absorption box 512, passes through the tightly filled activated carbon in the filler absorption box 512, and adsorbs organic matter and part of the acid gas in the tail gas, wherein the number of filler absorption boxes 512 can be set according to actual conditions; alkaline solution prepared by water, sodium hydroxide and other chemicals is added to the bottom of the spray tower 513 and the absorption liquid tank 514, and the lower part of the spray tower 513 is connected with the absorption liquid tank 514 and the connecting port is below the liquid level, such as Figure 7As shown, the air outlet of the spray tower 513 is located at the top of the spray tower. After the tail gas enters the spray tower 513, it goes directly to the induced draft device 52 without passing through the absorption liquid tank 514. The bottom of the spray tower 513 is connected to the absorption liquid tank 514 and the connecting port is below the liquid level. The spray pump 5131 transports the alkali solution in the absorption liquid tank 514 to the top of the spray tower 513 to form small droplets distributed over a large area. There are several layers of porous partitions 5132 in the spray tower 513, and hollow filler balls are distributed on each layer of porous partitions 513 (to increase the gas-liquid contact surface). The tail gas passes through the small droplets of alkali solution, the partitions adhering to the alkali solution, and the hollow filler balls adhering to the alkali solution from bottom to top, and is fully in contact with the alkali solution to remove the acidic substances therein. A feeding port is provided above the absorption liquid tank 514 for adding sodium hydroxide and other chemicals and observing the liquid level. A water inlet pipe and a float valve water level controller are provided on the upper side to replenish water when the liquid level drops. There is also an overflow pipe on the upper side to discharge the alkali solution when the liquid level is too high. A drain pipe and a drain valve are provided at the bottom of the side to discharge the alkali solution when the concentration of the absorbent in the alkali solution is too high. The exhaust gas treated by the exhaust gas treatment equipment 51 can be directly discharged into the air without causing air pollution.

[0053] To ensure that the exhaust gas discharged from the preparation chamber 41 and the lithium sulfide preparation device 1 can quickly flow through the above-mentioned absorption equipment 51 for purification and discharge; the exhaust gas treatment unit 5 also includes an induced draft device 52, and the induced draft device 52 includes an induced draft fan 521 and an exhaust chimney 522, and the air inlet of the induced draft fan 521 is connected to the air outlet of the spray tower 513; the exhaust chimney 522 is vertically arranged at the air outlet of the induced draft fan 521, and the air outlet of the exhaust chimney 522 is higher than the air outlet of the induced draft fan 521; the gas in the absorption equipment 51 is induced by the induced draft fan 521 to be discharged into the air at high altitude through the exhaust chimney 522, thereby reducing the impact on the surrounding environment.

[0054] In order to timely monitor the pH value of the liquid in the absorption liquid tank 514, when the liquid in the absorption liquid tank 514 cannot absorb hydrogen sulfide, timely replace or add products for absorbing hydrogen sulfide, such as sodium hydroxide, etc., the absorption liquid tank 514 is provided with a pH sensor 5141 for monitoring the pH value in the absorption liquid tank 514, and the induced draft fan 521 is provided with a flow meter 5211 for monitoring the gas flow rate, and the pH sensor 5141 and the flow meter 5211 are electrically connected to the parameter control system 2; by setting the pH sensor 5141 and the flow meter 5211 for real-time monitoring, when the gas flow rate of the induced draft fan 521 decays and the pH of the alkali solution in the absorption liquid tank 514 is lower than the set value and fed back to the parameter control system 2, the maintenance personnel check the induced draft fan 521 and add drugs to the absorption liquid tank 514 or replace the alkali solution in the absorption liquid tank 514 to ensure the normal operation of the exhaust gas treatment unit 5.

[0055] In order to facilitate unified control of the input of corresponding gases to the preparation chamber 41, the atmosphere purification module and the lithium sulfide preparation device 1, the closed system of the lithium sulfide preparation device also includes a gas control unit 3, the gas control unit 3 is arranged outside the preparation chamber 41, the gas control unit 3 includes a dry air storage tank 31, an inert gas storage tank 32 and a reducing gas storage tank 33, the output end of the dry air storage tank 31 is connected to the preparation chamber 41, the output end of the inert gas storage tank 32 is connected to the preparation chamber 41 and the lithium sulfide preparation device 1, the output end of the reducing gas storage tank 33 is connected to the input end of the atmosphere circulation module 44, the dry air storage tank 31, the inert gas storage tank 32 and the The reducing gas storage tank 33 is electrically connected to the parameter control system 2; the above-mentioned dry air storage tank 31 and inert gas storage tank 32 are connected to the preparation chamber 41 and the transition chamber 49 as needed, and a second working gas inlet valve 424 is provided between the dry air storage tank 31 and the preparation chamber 41 to control the input of dry air into the preparation chamber 41, and a dry air inlet valve 492 is provided between the dry air storage tank 31 and the transition chamber 49 to control the input of dry air into the transition chamber 49; a first working gas inlet valve 423 is provided between the inert gas storage tank 32 and the preparation chamber 41 to control the input of inert gas into the preparation chamber 41, and a second inert gas inlet valve 491 is provided between the inert gas storage tank 32 and the transition chamber 49 to control The inert gas is input into the transition chamber 49; the inert gas storage tank 32 is also connected to the lithium sulfide preparation device 1, and a first inert gas intake valve 11 is provided between the two to control the inert gas input into the lithium sulfide preparation device 1; the reducing gas storage tank 33 is connected to the atmosphere circulation module 44, and a reducing gas intake valve 443 is provided between the two to control the reducing gas input into the atmosphere circulation module 44; then the second working gas intake valve 424 and the dry air intake valve 492 on the dry air storage tank 31, the first working gas intake valve 423 and the second inert gas intake valve 491 on the inert gas storage tank 32, and the reducing gas intake valve 443 on the reducing gas storage tank 33 are connected one by one to the parameter control system 2 Electrically connected, the opening and closing of the second working gas intake valve 424, the dry air intake valve 492, the first working gas intake valve 423, the second inert gas intake valve 491, and the reducing gas intake valve 443 are controlled by the parameter control system 2. Specifically, the parameter control system 2 judges whether the corresponding gas needs to be input based on the monitoring values ​​fed back to the parameter control system 2 by various sensors arranged in the preparation chamber 41, such as the first air pressure sensor 421, the organic matter sensor 451, the first oxygen sensor 461, the water sensor 471, the hydrogen sulfide sensor 481, and the second oxygen sensor 494 arranged in the transition chamber 49, to thereby control the input of dry air, inert gas and reducing gas.

[0056] When dry air is used as the working gas in the preparation chamber 41, in order to ensure the dryness of the gas in the dry air storage tank 31 and to directly use outside air to save costs, a fourth air pump 311 is provided at the input end of the dry air storage tank 31, and a dehumidification device 312 is provided at the input end of the fourth air pump 311. The input end of the dehumidification device 312 is connected to the air, and an air intake valve 313 is provided at the input end of the dehumidification device 312, and the air intake valve 313 is electrically connected to the parameter control system 2; the outside air is controlled to enter the dehumidification device 312 for dehumidification through the air intake valve 313, and then input into the dry air storage tank 31 through the fourth air pump 311 and then into the preparation chamber 41, while ensuring the input and output pressures of the gas; such a setting can directly dehumidify the outside air and then directly input it into the preparation chamber 41 as dry air, which is less costly and easier to obtain than using inert gas as the sealed gas in the preparation chamber 41.

[0057] In order to facilitate the control of the amount of inert gas input into the lithium sulfide preparation device and save costs, a monitoring meter 111 for monitoring the pressure and flow rate of the inert gas is also provided between the inert gas storage tank 32 and the lithium sulfide preparation device 1. The monitoring meter 111 is electrically connected to the parameter control module. The gas pressure and flow rate of the inert gas are monitored in real time by the set monitoring meter 111, so as to complete the rapid replacement of the indoor atmosphere of the lithium sulfide preparation and meet the requirements of the normal preparation of lithium sulfide, thereby avoiding waste and saving costs.

[0058] The specific implementation modes of the present invention are further described below in conjunction with examples, but the present invention is not limited to the scope of the examples.

[0059] Embodiment 1:

[0060] Inert gas-argon gas is used as the working gas of the preparation chamber 41 and the transition chamber 49 and the internal protective gas of the lithium sulfide preparation device 1.

[0061] The air inlet of the transition chamber 49 is connected to the output end of the inert gas storage tank 32, and the inert gas-argon gas input into the transition chamber 49 is controlled by the second inert gas inlet valve 491; the first air pump 421 is connected to the output end of the inert gas storage tank 32 and the inert gas-argon gas input into the preparation chamber 41 is controlled by the first working gas inlet valve 423; the lithium sulfide preparation device 1 is placed in the preparation chamber 41, and the preparation chamber 41 and the transition chamber 49 are sealed; the lithium sulfide preparation device 1 is connected to the output end of the inert gas storage tank 32 and the inert gas-argon gas input into the lithium sulfide preparation device 1 is controlled by the first inert gas inlet valve 11, and then the tail gas emission pipe of the lithium sulfide preparation device 1 is connected to the air inlet of the sedimentation tank 511 in the tail gas treatment unit 5, and the tail gas emission of the lithium sulfide preparation device 1 is controlled by the first tail gas exhaust valve 12.

[0062] First, the first inert gas inlet valve 11 and the tail gas exhaust valve 12 of the preparation device are opened by using the parameter control system 2, the inert gas pressure and flow rate are specified and monitored by the monitoring meter 111 and fed back to the parameter control system 2, the gas in the lithium sulfide preparation device 1 is replaced, and the lithium sulfide preparation device 1 is filled with inert gas.

[0063] Then, the parameter control system 2 is used to open the first working gas intake valve 423, the first tail gas exhaust valve 427, the first inert gas intake valve 11, and the transition chamber exhaust valve 493, and the second working gas intake valve 424 and the dry air intake valve 492 of the transition chamber 49 are closed to replace the gas in the preparation chamber 41 and the transition chamber 49, and the water content is set to be no higher than 10ppm, the oxygen content is set to be no higher than 200ppm, and the gas pressure of the preparation chamber 41 and the transition chamber 49 is set to 100-500Pa; when the water sensor 471, the first oxygen sensor and the second oxygen sensor, the gas After the pressure sensor detects that the water content in the preparation chamber 41 and the transition chamber 49 is lower than 10ppm and the oxygen content is lower than 200ppm, it indicates that the replacement of the gases in the preparation chamber 41 and the transition chamber 49 has been completed, and the first working gas inlet valve 423, the first tail gas exhaust valve 427, the first inert gas inlet valve 11, and the transition chamber exhaust valve 493 are closed; at this time, the lithium sulfide preparation device 1 starts to prepare lithium sulfide, and the pressure in the preparation chamber 41 is set to 100-200Pa on the parameter control system 2, which is monitored by the pressure sensor and fed back to the parameter control system 2, and then the parameter control system 2 controls The air pressure control module 42 is turned on and off; the temperature in the preparation chamber 41 is set to 25-26°C on the parameter control system 2, which is monitored by the temperature sensor 431 and fed back to the parameter control system 2, and then the parameter control system 2 controls the opening and closing of the temperature control module 43; the parameter control system 2 controls the atmosphere circulation module 44 to be turned on, the third air pump 441 of the atmosphere circulation module 44, the third preparation chamber air inlet valve 444, the total atmosphere air inlet valve 446, the first atmosphere air inlet valve 454, the second atmosphere air inlet valve 464, and the third atmosphere air inlet valve 474 are turned on, and the third preparation chamber exhaust valve 445 , the reducing gas inlet valve 443 is closed, the organic matter control module 45, the oxygen control module 46, the moisture control module 47 and the hydrogen sulfide control module 48 are turned on, the second tail gas exhaust valve 485 and the third tail gas exhaust valve 476 are closed, so as to realize the atmosphere circulation purification in the preparation chamber 41; sodium hydroxide is added as the absorption liquid and the spray liquid in the absorption liquid tank 514 and the spray tower 513, a multi-layer staggered perforated baffle is arranged in the sedimentation tank 511, and the filler absorption box 512 is tightly filled with activated carbon, and then the parameter control system 2 is used to control the opening and closing of the induced draft equipment 52, thereby completing the preparation of lithium sulfide.

[0064] Embodiment 2:

[0065] Dry air is used as the working gas in the preparation chamber 41 and the transition chamber 49, and inert gas-argon is used as the internal protective gas of the lithium sulfide preparation device 1;

[0066] The air inlet of the transition chamber 49 is connected to the output end of the dry gas storage tank 31, and the inert gas-argon gas input to the transition chamber 49 is controlled by the dry air inlet valve 492; the first air pump 421 is connected to the output end of the dry gas storage tank 31 and the inert gas-argon gas input to the preparation chamber 41 is controlled by the second working gas inlet valve 424; the lithium sulfide preparation device 1 is placed in the preparation chamber 41, and the preparation chamber 41 and the transition chamber 49 are sealed; the lithium sulfide preparation device 1 is connected to the output end of the inert gas storage tank 32 and the inert gas-argon gas input to the lithium sulfide preparation device 1 is controlled by the first inert gas inlet valve 11, and then the tail gas emission pipe of the lithium sulfide preparation device 1 is connected to the air inlet of the sedimentation tank 511 in the tail gas treatment unit 5 and the tail gas emission of the lithium sulfide preparation device 1 is controlled by the first tail gas exhaust valve 12.

[0067] First, the parameter control system 2 is used to open the first inert gas inlet valve 11 and the tail gas exhaust valve 12 of the preparation device, and the inert gas pressure and flow rate are specified to replace the gas in the lithium sulfide preparation device 1 so that the lithium sulfide preparation device 1 is filled with inert gas.

[0068] Then, the air intake valve 313, the second working intake valve, the first tail gas exhaust valve 427, the dry air intake valve 492 and the transition chamber exhaust valve 493 are opened on the parameter control module, and the first working gas intake valve 423 and the second inert gas intake valve 491 of the transition chamber 49 are closed; the dehumidification equipment 312 and the fourth air pump 311 are opened to replace the gas in the preparation chamber 41 and the transition chamber 49, and the pressure in the preparation chamber 41 is set to 20-100 Pa on the parameter control system 2, which is monitored by the pressure sensor and fed back to the parameter control system 2, and then the parameter control system 2 controls the opening and closing of the air pressure control module 42; the temperature in the preparation chamber 41 is set to 24-25°C on the parameter control system 2, which is monitored by the temperature sensor 431 and fed back to the parameter control system 2, and then the parameter control system 2 controls the opening and closing of the temperature control module 43; the parameter control system 2 controls the opening of the atmosphere circulation module 44, and the atmosphere circulation module 45 is opened. The third air pump 441, the third preparation chamber air inlet valve 444, the total atmosphere air inlet valve 446, the first atmosphere air inlet valve 454, and the third atmosphere air inlet valve 474 of 44 are opened, the third preparation chamber exhaust valve 445 and the reducing gas air inlet valve 443 are closed, the organic matter control module 45, the moisture control module 47 and the hydrogen sulfide control module 48 are opened, the second atmosphere air inlet valve 464, the second tail gas exhaust valve 485, and the third tail gas exhaust valve 476 are closed, and the oxygen control module 46 is closed, so as to realize the atmosphere circulation purification in the preparation chamber 41; sodium hydroxide is added as the absorption liquid and the spray liquid in the absorption liquid tank 514 and the spray tower 513, a multi-layer staggered perforated baffle is set in the sedimentation box 511, and the filler absorption box 512 is tightly filled with activated carbon, and then the parameter control system 2 is used to control the opening and closing of the induced draft device 52, until the parameter control module observes that the water content of the atmosphere in the preparation chamber 41 is lower than 1ppm and the oxygen content is lower than 20ppm, and then the preparation of lithium sulfide is started.

Claims

1. A closed system for a lithium sulfide preparation device, comprising a lithium sulfide preparation device (1), characterized in that: The invention also comprises a closed unit (4), wherein the closed unit (4) comprises a preparation chamber (41) filled with dry gas and sealed, and an atmosphere purification module arranged in the preparation chamber (41); the lithium sulfide preparation device (1) is arranged in the preparation chamber (41); the lithium sulfide preparation device (1) is provided with an exhaust gas discharge pipe connected to the outside of the preparation chamber (41); the atmosphere purification module comprises an atmosphere circulation module (44), an organic matter control module (45), a hydrogen sulfide control module (48) and a moisture control module (47); the atmosphere circulation module (44) is connected to the organic matter control module (45) and the moisture control module (47) via an air supply pipe. (47), the organic matter control module (45) is connected to the hydrogen sulfide control module (48) through a gas pipe, the input end and the output end of the atmosphere circulation module (44) are both connected to the preparation chamber (41), the output end of the hydrogen sulfide control module (48) is connected to the preparation chamber (41) and the exhaust gas exhaust pipe, and the output end of the moisture control module (47) is connected to the preparation chamber (41) and the exhaust gas exhaust pipe; the atmosphere circulation module (44), the organic matter control module (45), the hydrogen sulfide control module (48) and the moisture control module (47) are electrically connected to a parameter control system (2).

2. The closed system of a lithium sulfide preparation device according to claim 1, characterized in that: The atmosphere purification module also includes an oxygen control module (46); the atmosphere circulation module (44), the oxygen control module (46) and the moisture control module (47) are connected in sequence via an air pipeline; and the oxygen control module (46) is electrically connected to the parameter control system (2).

3. A closed system for a lithium sulfide preparation device as claimed in claim 2, characterized in that: The atmosphere circulation module (44) comprises a third air pump (441) for introducing reducing gas; the organic matter control module (45) comprises an organic matter purification column (452) and an organic matter sensor (451) for monitoring the content of organic matter in the preparation chamber (41); the hydrogen sulfide control module (48) comprises a hydrogen sulfide purification column (482) and a hydrogen sulfide sensor (481) for monitoring the content of hydrogen sulfide in the preparation chamber (41); the moisture control module (47) comprises a water purification column (472) and a water sensor (471) for monitoring the moisture content in the preparation chamber (41); the oxygen control module (46) comprises an oxygen purification column (462) and a first oxygen sensor (461) for monitoring the oxygen content in the preparation chamber (41); the organic matter sensor (451), the hydrogen sulfide sensor (481), the water sensor (471) and the first oxygen sensor (461) are all electrically connected to the parameter control system (2); A third preparation chamber air inlet valve (444) is provided between the input end of the third air pump (441) and the preparation chamber (41); a first atmosphere air inlet valve (454) is provided between the output end of the third air pump (441) and the input end of the organic matter purification column (452); a second atmosphere air inlet valve (464) is provided between the output end of the third air pump (441) and the input end of the oxygen purification column (462); a third atmosphere air inlet valve (474) is provided between the output end of the third air pump (441) and the input end of the water purification column (472); the third air pump (441) is connected to the first atmosphere air inlet valve (454), the second atmosphere air inlet valve (464), and the third atmosphere air inlet valve (474). A total atmosphere inlet valve (446) is also provided between the gas valves (474); a third preparation chamber exhaust valve (445) is provided between the output end of the third air pump (441) and the preparation chamber (41); a second exhaust gas exhaust valve (485) is provided between the output end of the hydrogen sulfide purification column (482) and the exhaust gas discharge pipe, and a fourth preparation chamber exhaust valve (484) is provided between the output end of the hydrogen sulfide purification column (482) and the preparation chamber (41); a third exhaust gas exhaust valve (476) is provided between the output end of the water purification column (472) and the exhaust gas discharge pipe, and a fifth preparation chamber exhaust valve (475) is provided between the output end of the water purification column (472) and the preparation chamber (41); The third preparation chamber air inlet valve (444), the third preparation chamber exhaust valve (445), the fourth preparation chamber exhaust valve (484), the fifth preparation chamber exhaust valve (475), the total atmosphere air inlet valve (446), the first atmosphere air inlet valve (454), the second atmosphere air inlet valve (464), the third atmosphere air inlet valve (474), the second tail gas exhaust valve (485) and the third tail gas exhaust valve (476) are all electrically connected to the parameter control system.

4. A closed system for a lithium sulfide preparation device as claimed in claim 3, characterized in that: The organic matter purification column (452) is provided with a first heater (453); the hydrogen sulfide purification column (482) is provided with a fourth heater (483); the water purification column (472) is provided with a third heater (473); the oxygen purification column (462) is provided with a second heater (463); the first heater (453), the fourth heater (483), the third heater (473) and the second heater (463) are all electrically connected to the parameter control system (2).

5. The closed system of a lithium sulfide preparation device according to claim 1, characterized in that: The input end of the atmosphere circulation module (44) is also connected to a dust filter (442), and the input end of the dust filter (442) is connected to the preparation chamber (41).

6. The closed system of a lithium sulfide preparation device according to claim 1, characterized in that: An air pressure control module (42) is also provided in the preparation chamber (41); an input end of the air pressure control module (42) is connected to the preparation chamber (41); an output end of the air pressure control module (42) is connected to the preparation chamber (41) and an exhaust gas exhaust pipe; and the air pressure control module (42) is electrically connected to the parameter control system (2).

7. A closed system for lithium sulfide preparation device according to claim 6, characterized in that: The air pressure control module (42) comprises a first air pump (422) for introducing dry gas and a first air pressure sensor (421) for monitoring the air pressure in the preparation chamber (41); a first preparation chamber air inlet valve (425) is provided between the input end of the first air pump (422) and the preparation chamber (41); a first preparation chamber air exhaust valve (426) is provided between the output end of the first air pump (422) and the preparation chamber (41); and a first exhaust gas exhaust valve (427) is provided between the output end of the first air pump (422) and the exhaust gas exhaust pipe; the first air pressure sensor (421) is electrically connected to the parameter control system (2); and the first preparation chamber air inlet valve (425), the first preparation chamber exhaust valve (426), and the first exhaust gas exhaust valve (427) are all electrically connected to the parameter control system (2).

8. The closed system of a lithium sulfide preparation device according to claim 1, characterized in that: A temperature control module (43) is also provided in the preparation chamber (41), the input end and the output end of the temperature control module (43) are both connected to the preparation chamber (41), and the temperature control module (43) is electrically connected to the parameter control system (2).

9. A closed system for a lithium sulfide preparation device as claimed in claim 8, characterized in that: The temperature control module (43) comprises a temperature regulator (433), a second air pump (432) and a temperature sensor (431) for monitoring the temperature in the preparation chamber (41); the input end of the second air pump (432) is connected to the preparation chamber (41); the output end of the second air pump (432) is connected to the input end of the temperature regulator (433); the output end of the temperature regulator (433) is connected to the preparation chamber (41); a second preparation chamber air inlet valve (434) is provided between the input end of the second air pump (432) and the preparation chamber (41); a second preparation chamber exhaust valve (435) is provided between the output end of the temperature regulator (433) and the preparation chamber (41); the temperature regulator (433), the second air pump (432) and the temperature sensor (431) are electrically connected to the parameter control system (2); the second preparation chamber air inlet valve (434) and the second preparation chamber exhaust valve (435) are both electrically connected to the parameter control system (2).

10. The closed system of a lithium sulfide preparation device according to claim 1, characterized in that: A transition chamber (49) connected to the preparation chamber (41) is also provided on one side of the preparation chamber (41), and the transition chamber (49) is filled with dry gas.

11. A closed system for a lithium sulfide preparation device according to any one of claims 1 to 10, characterized in that: The invention also comprises a tail gas treatment unit (5) for treating exhaust gas from the preparation chamber (41) and the lithium sulfide preparation device (1); the tail gas treatment unit (5) is arranged outside the preparation chamber (41); the tail gas treatment unit (5) comprises an absorption device (51); and the absorption device (51) is connected to the tail gas discharge pipe.

12. The closed system of a lithium sulfide preparation device according to claim 11, characterized in that: The absorption device (51) comprises a sedimentation tank (511), a filler absorption tank (512), a spray tower (513) and an absorption liquid tank (514) which are connected in sequence, the air inlet of the sedimentation tank (511) is connected to the exhaust gas discharge pipe, the air outlet of the sedimentation tank (511) is connected to the air inlet of the filler absorption tank (512), the air outlet of the filler absorption tank (512) is connected to the air inlet of the spray tower (513), the lower part of the spray tower (513) is connected to the absorption liquid tank (514), and the air outlet of the spray tower (513) is connected to the external environment.

13. A closed system for lithium sulfide preparation device according to claim 12, characterized in that: The exhaust gas treatment unit (5) further comprises an induced draft device (52), wherein the induced draft device (52) comprises an induced draft fan (521) and an exhaust pipe (522), wherein an air inlet of the induced draft fan (521) is connected to an air outlet of the spray tower (513); and the exhaust pipe (522) is vertically arranged at the air outlet of the induced draft fan (521), and the air outlet of the exhaust pipe (522) is higher than the air outlet of the induced draft fan (521).

14. A closed system for lithium sulfide preparation device according to claim 13, characterized in that: The absorption liquid tank (514) is provided with a pH sensor (5141) for monitoring the pH value in the absorption liquid tank (514), and the induced draft fan (521) is provided with a flow meter (5211) for monitoring the gas flow rate. The pH sensor (5141) and the flow meter (5211) are electrically connected to the parameter control system (2).

15. A closed system for a lithium sulfide preparation device according to any one of claims 1 to 10, characterized in that: The invention also comprises a gas control unit (3), wherein the gas control unit (3) is arranged outside the preparation chamber (41), and the gas control unit (3) comprises a dry air storage tank (31), an inert gas storage tank (32) and a reducing gas storage tank (33); the output end of the dry air storage tank (31) is connected to the preparation chamber (41), the output end of the inert gas storage tank (32) is connected to the preparation chamber (41) and the lithium sulfide preparation device (1), the output end of the reducing gas storage tank (33) is connected to the input end of the atmosphere circulation module (44), and the dry air storage tank (31), the inert gas storage tank (32) and the reducing gas storage tank (33) are electrically connected to the parameter control system (2).

16. A closed system for lithium sulfide preparation device according to claim 15, characterized in that: The input end of the dry air storage tank (31) is provided with a fourth air pump (311), the input end of the fourth air pump (311) is provided with a dehumidification device (312), the input end of the dehumidification device (312) is connected to the air, the input end of the dehumidification device (312) is provided with an air intake valve (313), and the air intake valve (313) is electrically connected to the parameter control system (2).

17. The closed system of a lithium sulfide preparation device according to claim 15, characterized in that: A monitoring meter (111) for monitoring the pressure and flow rate of the inert gas is also provided between the inert gas storage tank (32) and the lithium sulfide preparation device (1), and the monitoring meter (111) is electrically connected to the parameter control system (2).

Images