Preparation system of bis (chlorosulfonyl) imide

Abstract

The utility model provides a preparation system of bis (chlorosulfonyl) imide. Under the condition that the mixing device and the homogenizing device in the preparation system of the bis (chlorosulfonyl) imide are matched for operation, a mixture of sulfamic acid and chlorosulfonic acid can be fully dispersed and mixed, so that slurry with good uniformity is obtained. As a result, the slurry prepared from sulfamic acid and chlorosulfonic acid can react with thionyl chloride efficiently and sufficiently. Therefore, according to the preparation system disclosed by the invention, the preparation raw materials of the bis (chlorosulfonyl) imide react after being fully mixed, so that the reaction time can be shortened, the conversion rate and the yield can be improved, and potential safety hazards caused by unsmooth circulation of the preparation raw materials in the pipeline can be reduced or even avoided.

Description

Technical Field

[0001] The present application relates to the field of preparation of bischlorosulfonyl imide, and in particular to a preparation system of bischlorosulfonyl imide. Background Art

[0002] In the lithium battery industry, lithium salt electrolyte is an important component of lithium batteries. Lithium bis(fluorosulfonyl)imide has broad application prospects due to its good performance in thermal stability, decomposition resistance and conductivity. Bis(chlorosulfonyl)imide is an important intermediate of lithium bis(fluorosulfonyl)imide, which affects the yield of lithium bis(fluorosulfonyl)imide. In a typical scheme, bis(chlorosulfonyl)imide is synthesized by chlorination reaction using aminosulfonic acid and chlorosulfonic acid. However, aminosulfonic acid and chlorosulfonic acid are solid and liquid phases respectively under normal temperature and pressure conditions. The uniformity of the slurry formed by the mixture of the two will significantly affect the mass transfer and heat transfer effect of the chlorination reaction, thereby affecting the reaction time, conversion rate and yield. In addition, the uniformity of the slurry also affects the smoothness of the slurry flow in the heat exchange equipment and pipelines. Since aminosulfonic acid is highly corrosive and has a strong exothermic reaction when in contact with water, producing thick smoke or even explosion, if the uniformity of the slurry is poor, the dispersion effect is poor, which may cause pipeline blockage, which may pose a safety hazard. Utility Model Content

[0003] This application is made in view of the state of the prior art. The purpose of this application is to provide a system for preparing bischlorosulfonyl imide, which can achieve the reaction of the raw materials for preparing bischlorosulfonyl imide after being fully mixed, thereby improving the reaction time, conversion rate and yield, and reducing or even avoiding the safety hazards caused by the poor circulation of the raw materials for preparing.

[0004] In order to achieve the above objectives, this application adopts the following technical solutions.

[0005] The present application provides a system for preparing bischlorosulfonyl imide, comprising: a mixing device, comprising a first inlet and a first outlet, and used for mixing aminosulfonic acid and chlorosulfonic acid; a homogenizing device, comprising a second inlet and a second outlet, wherein the second inlet is connected to the first outlet, and the second outlet is connected to the first inlet, and the mixture in the mixing device is cyclically emulsified or cyclically dispersed via the homogenizing device; and a reaction device, which is connected to the mixing device and receives the mixture, and the mixture reacts with thionyl chloride in the reaction device to generate bischlorosulfonyl imide.

[0006] In an optional solution, it further includes a metering device, which is connected to the mixing device to meter the aminosulfonic acid to be transported; and / or, it also includes a feeding device, which is connected to the mixing device to transport the aminosulfonic acid into the mixing device.

[0007] In another optional solution, the metering device comprises a silo and a weight sensor, the outlet of the silo is communicated with the mixing device, and the weight sensor is installed in the silo and is used to sense the weight of aminosulfonic acid added to the silo.

[0008] In another optional solution, the preparation system further includes a first flow sensor and a control valve, wherein the control valve is opened and closed based on parameters detected by the first flow sensor, and the first flow sensor is used to sense the flow rate of chlorosulfonic acid delivered to the mixing device.

[0009] In another optional solution, the homogenizing device includes an emulsifying pump and an emulsifying motor, the inlet of the emulsifying pump is connected to the first outlet of the mixing device and the outlet is connected to the first inlet of the mixing device, and the emulsifying motor is transmission-connected to the emulsifying pump; or the homogenizing device includes an online dispersing device.

[0010] In another optional solution, a second flow sensor is further included, and the emulsification motor is turned on and off based on parameters detected by the second flow sensor, and the second flow sensor is used to sense the flow of the mixture flowing from the outlet of the emulsification pump to the mixing device.

[0011] In another optional scheme, the mixing device includes a mixing kettle, a disperser and a stirrer motor, the mixing kettle is used to contain aminosulfonic acid and chlorosulfonic acid, the disperser is transmission-connected to the stirrer motor; and / or the stirring speed of the mixing device is 200 rpm to 500 rpm.

[0012] In another optional scheme, it also includes a material transfer device, which is connected between the mixing device and the reaction device. The material transfer device includes a material transfer device and a material transfer motor. The inlet of the material transfer device is connected to the first outlet of the mixing device and the outlet is connected to the reaction device. The material transfer motor is transmission-connected to the material transfer device.

[0013] In another optional scheme, a third flow sensor is further included, and the material transfer motor is opened and closed based on the parameters detected by the third flow sensor. The third flow sensor is used to sense the flow rate of the mixture flowing from the outlet of the material transfer device to the reaction device; and / or the first outlet of the mixing device is always connected to the material transfer device.

[0014] In another optional solution, the mixing device and the homogenizing device are arranged in groups, and at least two groups are arranged in parallel with each other.

[0015] By adopting the above technical scheme, the present application provides a preparation system of bischlorosulfonyl imide. In the preparation system of the bischlorosulfonyl imide, a mixing device, a homogenizing device (such as an emulsifying device or an online dispersing device) and a reaction device are included. The mixing device is used to mix aminosulfonic acid and chlorosulfonic acid. The second inlet of the homogenizing device is connected to the first outlet of the mixing device and the second outlet is connected to the first inlet of the mixing device, so that the mixture from the mixing device is circulated emulsified or dispersed via the homogenizing device. The mixing device is also connected to the reaction device, so that the mixture from the mixing device is transported to the reaction device and reacts with thionyl chloride in the reaction device to generate bischlorosulfonyl imide.

[0016] In this way, when the mixing device and the homogenizing device cooperate to operate, the mixture of aminosulfonic acid and chlorosulfonic acid can be fully dispersed and mixed to obtain a slurry with good uniformity. Thus, the slurry prepared by aminosulfonic acid and chlorosulfonic acid can react efficiently and fully with thionyl chloride. Thus, according to the preparation system of the present application, the raw materials for preparing bischlorosulfonyl imide are reacted after being fully mixed, thereby shortening the reaction time, improving the conversion rate and yield, and reducing or even avoiding the potential safety hazards caused by the poor circulation of the raw materials in the pipeline. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 Schematic diagram showing the topological structure of a system for preparing bischlorosulfonyl imide according to the first embodiment of the present application.

[0018] Figure 2 Schematic diagram showing the topological structure of a system for preparing bischlorosulfonyl imide according to the second embodiment of the present application.

[0019] Description of Reference Numerals

[0020] 1 mixing device; 11 mixing kettle; 12 dispersing stirrer; 13 stirrer motor;

[0021] 2 emulsification device; 21 emulsification pump; 22 emulsification motor;

[0022] 3 material transfer device; 31 material transfer device; 32 material transfer motor;

[0023] 4. Reaction device;

[0024] 5. Feeding device;

[0025] 6 metering device; 61 silo; 62 weight sensor;

[0026] FC1 is the first flow sensor; FC2 is the second flow sensor; FC3 is the third flow sensor; V is the control valve. DETAILED DESCRIPTION

[0027] The exemplary embodiments of the present application are described below with reference to the accompanying drawings. It should be understood that these specific descriptions are only used to teach those skilled in the art how to implement the present application, and are not intended to exhaust all feasible methods of the present application, nor to limit the scope of the present application.

[0028] In this application, unless otherwise specified, the connection between two objects (including but not limited to between devices) means that the inlet of one object is connected to the outlet of another object, and the connection may or may use some pipelines or conduits. In the figure, the arrow on the connecting line representing the pipeline or conduit shows the flow direction of the fluid in the pipeline or conduit.

[0029] In the present application, unless otherwise specified, the "opening and closing" of the control valve includes the control valve being fully opened, the control valve being fully closed, and the control valve opening being controllably adjustable; the "opening and closing" of the motor includes the open state in which the motor is operating at various required powers and the closed state in which the motor is not operating. In addition, variable frequency motors such as emulsifying motors and material transfer motors can also control the opening of pipelines or pipelines, thereby controlling the flow rate of fluids in the pipelines or pipelines.

[0030] In the present application, unless otherwise specified, "drive connection" refers to a connection between two components that can transmit driving force / driving torque, including direct connection and indirect connection.

[0031] The following describes a system for preparing bischlorosulfonyl imide according to the first embodiment of the present application in conjunction with the accompanying drawings.

[0032] (System for preparing bischlorosulfonyl imide according to the first embodiment of the present application)

[0033] like Figure 1 As shown, the preparation system of bischlorosulfonyl imide according to the first embodiment of the present application includes a mixing device 1, an emulsifying device (homogenizing device) 2, a material transfer device 3, a reaction device 4, a feeding device 5 and a metering device 6. The mixing device 1 is connected to the feeding device 5 via the metering device 6 to receive the aminosulfonic acid from the feeding device 5, and can receive the corresponding amount of chlorosulfonic acid, and then the aminosulfonic acid and chlorosulfonic acid added to the mixing device 1 are stirred and mixed. The inlet of the emulsifying device 2 is connected to the bottom of the mixing device 1 and the outlet is connected to the top of the mixing device 1, so that the mixture (slurry) of aminosulfonic acid and chlorosulfonic acid in the mixing device 1 can be circulated and emulsified via the emulsifying device 2. The material transfer device 3 is connected to both the mixing device 1 and the reaction device 4, so that the material transfer device 3 can transport the mixture from the mixing device 1 to the reaction device 4 to react with thionyl chloride in the reaction device 4 to generate bischlorosulfonyl imide. Thus, the preparation system of bischlorosulfonyl imide according to the first embodiment of the present application can achieve intermittent reaction.

[0034] In this embodiment, if Figure 1As shown, the mixing device 1 includes a mixing kettle 11, a dispersing stirrer 12 and a stirrer motor 13, and the mixing kettle 11 includes a first inlet and a first outlet and is used to receive and hold aminosulfonic acid and chlorosulfonic acid. The working conditions of the mixing kettle 11 are normal temperature and pressure conditions, and the energy consumption is low. The dispersing stirrer 12 is arranged in the mixing kettle 11 and is connected to the stirrer motor 13 outside the mixing kettle 11. When the stirrer motor 13 is powered on, the rotor of the stirrer motor 13 can drive the dispersing stirrer 12, so that the dispersing stirrer 12 can stir the mixture of aminosulfonic acid and chlorosulfonic acid in the mixing kettle 11 with a stirring speed (rotating speed) of 200rpm to 500rpm (wherein rpm represents revolutions per minute), and the stirring lasts for 0.5h to 1h (wherein h represents hours). In this way, the stirring speed (rotation speed) and shear line speed of the liquid and solid phases (aminosulfonic acid and chlorosulfonic acid) in the mixing kettle 11 can be increased, and the collision and disturbance between the two raw materials, between the raw materials and the disperser 12, and between the raw materials and the wall of the mixing kettle 11 can be enhanced, making it easier for the mixture to form a slurry in which the two raw materials are evenly dispersed.

[0035] In this embodiment, if Figure 1 As shown, the emulsifying device 2 includes a second inlet and a second outlet, the second inlet is connected to the first outlet of the mixing kettle 11 of the mixing device 1, and the second outlet is connected to the second outlet of the mixing kettle 11 of the mixing device 1. Thus, the second inlet and the second outlet of the emulsifying device 2 are both connected to the mixing device 1, so that the mixture from the mixing device 1 can be circulated and emulsified through the emulsifying device 2. The emulsifying device 2 includes an emulsifying pump 21 and an emulsifying motor 22. The inlet of the emulsifying pump 21 is connected to the first outlet located at the bottom of the mixing kettle 11, and the outlet is connected to the first inlet located at the top of the mixing kettle 11. The emulsifying pump 21 can extract the slurry from the bottom of the mixing kettle 11 of the mixing device 1. The emulsifying motor 22 is a variable frequency motor, and the emulsifying motor 22 is transmission-connected to the emulsifying pump 21. When the emulsifying motor 22 is powered, the rotor of the emulsifying motor 22 drives the rotor of the emulsifying pump 21 to rotate at a high speed, thereby utilizing the rotor of the emulsifying pump 21 to shear, squeeze, collide and crush the raw materials, thereby enhancing the mixing uniformity of the raw materials, and allowing the emulsifying pump 21 to emulsify the mixed slurry to further improve the mixing uniformity of the raw materials, thereby making one raw material evenly dispersed in another raw material in the form of extremely small particles / droplets, thereby obtaining a slurry with better uniformity. The slurry in the mixing device 1 can be cyclically emulsified multiple times (for example, 3 to 4 times) by the emulsifying device 2, and the number of cyclic emulsifications can be adjusted as needed.

[0036] In this embodiment, if Figure 1As shown, the material transfer device 3 is connected between the mixing device 1 and the reaction device 4. Specifically, the material transfer device 3 is directly connected to the mixing device 1, and is used to convey the emulsified mixture in the mixing device 1. The material transfer device 3 includes a material transfer device 31 and a material transfer motor 32. The material transfer device 31 can be a screw conveyor or other equipment with a conveying function. The inlet of the material transfer device 31 is always connected to the first outlet at the bottom of the mixing kettle 11, and the outlet is connected to the reaction device 4. The material transfer motor 32 is a variable frequency motor, and the material transfer motor 32 is transmission-connected with the material transfer device 31, so that the material transfer motor 32 can drive the material transfer device 31 to convey the mixture in the mixing kettle 11 to the reaction device 4. The material transfer device 3 and the mixing device 1 are always connected without a control valve. The opening and closing of the material transfer motor 32 can achieve the same function as the opening and closing of the control valve, that is, controlling the amount of the mixture (slurry) conveyed, avoiding the reduction of the channel cross-section of the pipeline or pipeline caused by the adjustment of the control valve, thereby reducing the risk of blockage of the pipeline or pipeline of the system and causing corrosion and safety problems.

[0037] In this embodiment, if Figure 1 As shown, the reaction device 4 is connected to the material transfer device 3, so that the material transfer device 3 can transport the mixture from the mixing device 1 to the reaction device 4, so as to react with thionyl chloride in the reaction device 4 to generate bis(chlorosulfonyl)imide. It can be understood that the reaction device 4 includes a reaction vessel with adjustable reaction pressure, and the inlet of the reaction vessel is connected to the outlet of the material transfer device 31 of the material transfer device 3. The reaction vessel can be various containers that can smoothly realize the safe and smooth progress of the above-mentioned chemical reaction, such as a reaction kettle, a reactor, a generator, a synthesis tower, etc.

[0038] In this embodiment, if Figure 1 As shown, the feeding device 5 is connected to the mixing device 1 via the metering device 6, so that the aminosulfonic acid from the feeding device 5 is transported to the mixing device 1 after being measured by the metering device 6. The feeding device 5 can be an automatic feeding machine. The metering device 6 includes a silo 61 and a weight sensor 62. The inlet of the silo 61 is connected to the feeding device 5, and the outlet of the silo 61 is connected to the mixing kettle 11 of the mixing device 1. The weight sensor 62 is installed in the silo 61 and is used to sense the weight of the aminosulfonic acid in the solid state added to the silo 61. In this way, not only can the automatic feeding process be completed by the automatic feeding machine, but also the aminosulfonic acid after accurate measurement can be transported to the mixing kettle 11 by the metering device 6, and then the operation process of the automatic feeding machine can be controlled by the metering data fed back by the metering device 6.

[0039] In addition, in this embodiment, Figure 1As shown, the preparation system includes a first flow sensor FC1 and a control valve V. The control valve V and the first flow sensor FC1 can be electrically connected or signal connected, so that the control valve V is opened and closed based on the parameters detected by the first flow sensor FC1. The first flow sensor FC1 is used to sense the flow rate of liquid-phase chlorosulfonic acid delivered to the mixing device 1. In this way, the precise feeding of chlorosulfonic acid can be achieved by using this locking control. It can be understood that the electrical connection or signal connection can be indirectly achieved through a controller. The electrical connection or signal connection described in this article can be achieved in the same way, and will not be repeated below.

[0040] Furthermore, the preparation system further includes a second flow sensor FC2. The second flow sensor FC2 can be electrically connected or signal connected to the emulsification motor 22, so that the emulsification motor 22 is turned on and off based on the parameters detected by the second flow sensor FC2. The second flow sensor FC2 is used to sense the flow rate of the slurry flowing from the outlet of the emulsification pump 21 to the mixing kettle 11 of the mixing device 1. In this way, the amount of the emulsified slurry can be accurately controlled by this control.

[0041] Furthermore, the preparation system further includes a third flow sensor FC3. The third flow sensor FC3 can be electrically connected or signal connected to the material transfer motor 32, so that the material transfer motor 32 is turned on and off based on the parameters detected by the third flow sensor FC3. The third flow sensor FC3 is used to sense the flow rate of the mixture flowing from the outlet of the material transfer device 31 to the reaction device 4. In this way, the amount of slurry delivered to the reaction device 4 can be accurately controlled by using this control.

[0042] The following describes a system for preparing bischlorosulfonyl imide according to a second embodiment of the present application.

[0043] (System for preparing bischlorosulfonyl imide according to the second embodiment of the present application)

[0044] like Figure 2 As shown, the system for preparing bischlorosulfonyl imide according to the second embodiment of the present application includes all the devices and connecting pipelines of the system for preparing bischlorosulfonyl imide according to the first embodiment of the present application, and is also provided with an additional structure. The following mainly describes the differences between the two.

[0045] In this embodiment, different from the first embodiment, as Figure 2As shown, two identical subsystems are arranged corresponding to the same material transfer device 3, and each subsystem includes a mixing device 1, an emulsifying device 2, a metering device 6 and a feeding device 5, as well as sensors and control valves corresponding to these devices. The two subsystems are independent of each other and are connected in parallel in the preparation system. Moreover, in each subsystem, the mixing device 1 and the emulsifying device 2 are arranged in groups in cooperation with each other, and the mixing devices 1 in the two subsystems are all connected to the same material transfer device 3. Further, a corresponding control valve (not shown) can be arranged between the mixing device 1 and the material transfer device 3 of each subsystem, so that the mixture (slurry) of aminosulfonic acid and chlorosulfonic acid can be continuously transported into the reaction device 4 via the material transfer device 3 through the two subsystems, thereby enabling the entire preparation system to realize continuous supply into the reaction device 4. In the case where the reaction device 4 is used as a continuous reaction device, the preparation system according to the present embodiment can perform continuous reaction. It can be understood that in other optional schemes, the mixing devices 1 in the two subsystems can also be respectively connected to different material transfer devices 3, and at this time, different material transfer devices 3 are all connected to the same reaction device 4.

[0046] It should be understood that the above embodiments are merely exemplary and are not intended to limit the present application. Those skilled in the art may make various modifications and changes to the above embodiments under the guidance of the present application without departing from the scope of the present application. Further, the following supplementary explanations are provided.

[0047] i. In a variation of the second embodiment above, more sets of subsystems connected in parallel may be provided to continuously supply sufficient raw materials.

[0048] ii. In the variations of the first and second embodiments above, an online dispersion device may be used instead of the emulsification device 2 as a homogenization device, which can achieve the same technical effect.

[0049] iii. It can be understood that in the above modification of the first embodiment, only one of the feeding device 5 and the metering device 6 can be provided. In the case where only the feeding device 5 is provided, the feeding device 5 can be directly connected to the mixing device 1 to transport the aminosulfonic acid into the mixing device 1. In this case, the aminosulfonic acid in the feeding device 5 can be metered by a metering device outside the preparation system. In the case where only the metering device 6 is provided, the metering device 6 can be directly connected to the mixing device 1, and the transported aminosulfonic acid is transported to the mixing device 1 after being metered by the metering device 6. In this case, the metering device plays the role of both metering and feeding.

[0050] Iv. in the preparation system of bischlorosulfonyl imide of the present application, adopt dispersion and emulsification process, utilize efficient dispersing stirrer 12 and supporting external circulation emulsifying device 2 in mixing device 1, rapidly and uniformly disperse solid and liquid two-phase raw materials (aminosulfonic acid and chlorosulfonic acid). Moreover, the particle size of solid raw materials is also reduced, specifically can be reduced to micron level (for example, particle size is 40 microns to 80 microns), so it is helpful to increase the surface area of ​​liquid-solid phase raw material reaction, thereby improving reaction conversion rate, and promoting the production efficiency of bischlorosulfonyl imide. In addition, after slurry is dispersed and emulsified system, uniformity is significantly improved, and there is no problem of particle agglomeration and clogging caused by solid accumulation or liquid phase encapsulation in the preparation system, and there is no local overheating phenomenon caused by uneven heat transfer, and the possibility of potential safety hazards is reduced.

Claims

1. A system for preparing bischlorosulfonyl imide, characterized in that: include: a mixing device, comprising a first inlet and a first outlet, and for mixing sulfamic acid and chlorosulfonic acid; A homogenizing device, comprising a second inlet and a second outlet, wherein the second inlet is connected to the first outlet, and the second outlet is connected to the first inlet, and the mixture in the mixing device is cyclically emulsified or cyclically dispersed via the homogenizing device; as well as A reaction device is connected to the mixing device and receives the mixture. The mixture reacts with thionyl chloride in the reaction device to generate bischlorosulfonyl imide.

2. The system for preparing bischlorosulfonyl imide according to claim 1, characterized in that: Also includes a metering device, the metering device is connected to the mixing device to meter the aminosulfonic acid to be delivered; and / or, The invention also comprises a feeding device, which is communicated with the mixing device and is used for conveying aminosulfonic acid into the mixing device.

3. The system for preparing bischlorosulfonyl imide according to claim 2, characterized in that: The metering device comprises a silo and a weight sensor. The outlet of the silo is communicated with the mixing device. The weight sensor is installed in the silo and is used to sense the weight of aminosulfonic acid added to the silo.

4. The system for preparing bischlorosulfonyl imide according to claim 1, characterized in that: The preparation system further includes a first flow sensor and a control valve, wherein the control valve is opened and closed based on a parameter detected by the first flow sensor, and the first flow sensor is used to sense the flow of chlorosulfonic acid delivered to the mixing device.

5. The system for preparing bischlorosulfonyl imide according to any one of claims 1 to 4, characterized in that: The homogenizing device comprises an emulsifying pump and an emulsifying motor, the inlet of the emulsifying pump is communicated with the first outlet of the mixing device and the outlet is communicated with the first inlet of the mixing device, and the emulsifying motor is drivingly connected to the emulsifying pump; or The homogenizing device comprises an online dispersing device.

6. The system for preparing bischlorosulfonyl imide according to claim 5, characterized in that: A second flow sensor is further included. The emulsifying motor is turned on and off based on a parameter detected by the second flow sensor. The second flow sensor is used to sense the flow rate of the mixture flowing from the outlet of the emulsifying pump to the mixing device.

7. The system for preparing bischlorosulfonimide according to any one of claims 1 to 4, characterized in that: The mixing device comprises a mixing kettle, a dispersing agitator and a stirrer motor, wherein the mixing kettle is used to contain aminosulfonic acid and chlorosulfonic acid, and the dispersing agitator is drivingly connected to the stirrer motor; and / or, The stirring speed of the mixing device is 200 rpm to 500 rpm.

8. The system for preparing bischlorosulfonyl imide according to any one of claims 1 to 4, characterized in that: It also includes a material transfer device, which is connected between the mixing device and the reaction device. The material transfer device comprises a material transfer device and a material transfer motor. The inlet of the material transfer device is connected with the first outlet of the mixing device and the outlet is connected with the reaction device. The material transfer motor is transmission-connected with the material transfer device.

9. The system for preparing bischlorosulfonyl imide according to claim 8, characterized in that: It also includes a third flow sensor, the material transfer motor is turned on and off based on the parameters detected by the third flow sensor, and the third flow sensor is used to sense the flow of the mixture flowing from the outlet of the material transfer device to the reaction device; and / or The first outlet of the mixing device is always connected with the material transfer device.

10. The system for preparing bischlorosulfonimide according to any one of claims 1 to 4, characterized in that: The mixing device and the homogenizing device are arranged in groups, and at least two groups are arranged in parallel with each other.

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