CN222434171U - Preparation system of dichloro-sulfonyl imide - Google Patents

Abstract

The application provides a system for preparing dichloro sulfonyl imide. When the mixing device and the homogenizing device in the system for producing the bischlorosulfimide are operated in combination, the sulfamic acid and chlorosulfonic acid mixture can be sufficiently dispersed and mixed to obtain a slurry with good uniformity. Thus, the slurry prepared from sulfamic acid and chlorosulfonic acid can be efficiently and sufficiently reacted with thionyl chloride. Therefore, the preparation system provided by the application realizes that the preparation raw materials of the dichloro sulfimide react after being fully mixed, so that the reaction time can be shortened, the conversion rate and the yield can be improved, and the potential safety hazard caused by unsmooth circulation of the preparation raw materials in a pipeline can be reduced or even avoided.

Description

Preparation system of dichloro-sulfonyl imide

Technical Field

The application relates to the field of preparation of dichloro sulfonyl imide, in particular to a system for preparing dichloro sulfonyl imide.

Background

In the lithium battery industry, lithium salt electrolyte is an important component of a lithium battery, and lithium bis (fluorosulfonyl) imide has a wide application prospect due to good performance in the aspects of thermal stability, decomposition resistance and conductivity. The dichlorsulfimide is an important intermediate of the lithium bisfluorosulfonimide, and influences the yield of the lithium bisfluorosulfonimide. In a typical scheme, sulfamic acid and chlorosulfonic acid are utilized for chlorination reaction to synthesize dichlorosulfimide, but the sulfamic acid and chlorosulfonic acid are respectively in a solid phase and a liquid phase under normal temperature and normal pressure, and the uniformity of slurry formed by mixing the sulfamic acid and the chlorosulfonic acid can obviously influence the mass transfer effect and the heat transfer effect of the chlorination reaction, thereby influencing the reaction time, the conversion rate and the yield. In addition, the uniformity of the slurry also affects the smoothness of the slurry flow in the heat exchange equipment and the pipeline. Since sulfamic acid has strong corrosiveness and generates strong exothermic reaction when contacting water, dense smoke and even explosion are generated, if the uniformity of slurry is poor, the dispersing effect is poor, the pipeline can be blocked, and thus, potential safety hazards can exist.

Disclosure of utility model

The present application has been made in view of the above state of the art. The application aims to provide a system for preparing dichlorsulfoximine, which can realize that the raw materials for preparing dichlorsulfoximine react after being fully mixed, thereby improving the reaction time, the conversion rate and the yield, and reducing or even avoiding the potential safety hazard caused by unsmooth flow of the raw materials for preparing.

In order to achieve the above object, the present application adopts the following technical scheme.

The application provides a preparation system of dichlor sulfimide, which comprises a mixing device, a homogenizing device and a reaction device, wherein the mixing device comprises a first inlet and a first outlet and is used for mixing sulfamic acid and chlorosulfonic acid, the homogenizing device comprises a second inlet and a second outlet, the second inlet is connected with the first outlet, the second outlet is connected with the first inlet, a mixture in the mixing device is circularly emulsified or circularly dispersed through the homogenizing device, and the reaction device is communicated with the mixing device and receives the mixture, and the mixture and thionyl chloride react in the reaction device to generate dichlor sulfimide.

In an alternative, the device further comprises a metering device which is communicated with the mixing device to meter the conveyed sulfamic acid, and/or a feeding device which is communicated with the mixing device and is used for conveying the sulfamic acid into the mixing device.

In another alternative, the metering device comprises a silo and a weight sensor, the outlet of the silo is in communication with the mixing device, and the weight sensor is mounted to the silo and is used for sensing the weight of sulfamic acid added to the silo.

In another alternative, the preparation system further comprises a first flow sensor for sensing the flow of chlorosulfonic acid delivered into the mixing device and a control valve that opens and closes based on a parameter detected by the first flow sensor.

In another alternative, the homogenizing device comprises an emulsifying pump and an emulsifying motor, wherein the inlet of the emulsifying pump is communicated with the first outlet of the mixing device, the outlet of the emulsifying pump is communicated with the first inlet of the mixing device, and the emulsifying motor is in transmission connection with the emulsifying pump, or the homogenizing device comprises an online dispersing device.

In another alternative, the emulsifying motor is further provided with a second flow sensor, which is opened and closed based on a parameter detected by the second flow sensor, and the second flow sensor is used for sensing the flow rate of the mixture flowing from the outlet of the emulsifying pump to the mixing device.

In another alternative, the mixing device includes a mixing kettle for containing sulfamic acid and chlorosulfonic acid, a dispersing agitator drivingly coupled to the agitator motor, and/or an agitator motor, and/or the mixing device has an agitation speed of 200rpm to 500rpm.

In another alternative scheme, the device further comprises a material transferring device, wherein the material transferring device is connected between the mixing device and the reaction device, the material transferring device comprises a material transferring device and a material transferring motor, an inlet of the material transferring device is communicated with a first outlet of the mixing device, an outlet of the material transferring device is communicated with the reaction device, and the material transferring motor is in transmission connection with the material transferring device.

In another alternative, the device further comprises a third flow sensor, wherein the material transferring motor is opened and closed based on the parameter detected by the third flow sensor, the third flow sensor is used for sensing the flow rate of the mixture flowing from the outlet of the material transferring device to the reaction device, and/or the first outlet of the mixing device is always communicated with the material transferring device.

In another alternative, the mixing device and the homogenizing device are arranged in groups and at least two groups are arranged in parallel to each other.

By adopting the technical scheme, the application provides a system for preparing dichloro sulfonyl imide. The system for producing the bischlorosulfimide comprises a mixing device, a homogenizing device (such as an emulsifying device or an online dispersing device) and a reaction device. The mixing device is used for mixing sulfamic acid and chlorosulfonic acid. The second inlet of the homogenizing device is in communication with the first outlet of the mixing device and the second outlet is in communication with the first inlet of the mixing device such that the mixture from the mixing device is cyclically emulsified or cyclically dispersed via the homogenizing device. The mixing device is also communicated with the reaction device, so that the mixture from the mixing device is conveyed to the reaction device and reacts with thionyl chloride in the reaction device to generate the dichloro-sulfonyl imide.

In this way, when the mixing device and the homogenizing device are operated in combination, the sulfamic acid and chlorosulfonic acid mixture can be sufficiently dispersed and mixed to obtain a slurry with good uniformity. Thus, the slurry prepared from sulfamic acid and chlorosulfonic acid can be efficiently and sufficiently reacted with thionyl chloride. Therefore, the preparation system provided by the application realizes that the preparation raw materials of the dichloro sulfimide react after being fully mixed, so that the reaction time can be shortened, the conversion rate and the yield can be improved, and the potential safety hazard caused by unsmooth circulation of the preparation raw materials in a pipeline can be reduced or even avoided.

Drawings

Fig. 1 is a schematic diagram showing the topology of a system for producing bischlorosulfonimide according to the first embodiment of the present application.

Fig. 2 is a schematic diagram showing the topology of a system for producing bischlorosulfonimide according to a second embodiment of the present application.

Description of the reference numerals

1 A mixing device, 11 a mixing kettle, 12 a dispersing stirrer and 13 a stirrer motor;

2, an emulsifying device, 21, an emulsifying pump and 22, an emulsifying motor;

3, a material transferring device; a 31 material transferring device, a 32 material transferring motor;

4. A reaction device;

5. A feeding device;

6 metering device, 61 stock bin, 62 weight sensor;

FC1 first flow sensor, FC2 second flow sensor, FC3 third flow sensor, and V control valve.

Detailed Description

Exemplary embodiments of the present application are described below with reference to the accompanying drawings. It should be understood that these specific illustrations are for the purpose of illustrating how one skilled in the art may practice the application, and are not intended to be exhaustive of all of the possible ways of practicing the application, nor to limit the scope of the application.

In the present application, unless specifically stated otherwise, communication between two objects (including but not limited to between devices) means that the inlet of one object and the outlet of the other object are in communication with each other, which communication may or may not use some lines or pipes. In the figures, arrows on the lines representing the lines or pipes show the direction of flow of the fluid in the lines or pipes.

In the present application, the "opening and closing" of the control valve includes the complete opening of the control valve, the complete closing of the control valve and the controllable adjustment of the opening of the control valve, and the "opening and closing" of the motor includes the open state in which the motor operates at various required powers and the closed state in which the motor does not operate, and in addition, the variable frequency motor such as the emulsification motor and the inversion motor can also control the opening of the pipeline or the piping, thereby controlling the flow rate of the fluid in the pipeline or the piping, unless otherwise specified.

In the present application, unless otherwise specified, "drive coupling" refers to a connection between two components capable of transmitting a driving force/driving torque, and includes direct connection and indirect connection.

The following describes a system for producing bischlorosulfonimide according to the first embodiment of the present application with reference to the drawings.

(Preparation System of bischlorosulfonimide according to the first embodiment of the application)

As shown in fig. 1, the production system of a bischlorosulfonimide according to the first embodiment of the application comprises a mixing device 1, an emulsifying device (homogenizing device) 2, a material transferring device 3, a reaction device 4, a material feeding device 5, and a metering device 6. The mixing device 1 communicates with the dosing device 5 via a metering device 6 to receive sulfamic acid from the dosing device 5 and is capable of receiving a corresponding amount of chlorosulfonic acid to thereby stir and mix the sulfamic acid and chlorosulfonic acid added to the mixing device 1. The inlet of the emulsifying device 2 communicates with the bottom of the mixing device 1 and the outlet communicates with the top of the mixing device 1, so that the mixture (slurry) of sulfamic acid and chlorosulfonic acid inside the mixing device 1 can be cyclically emulsified via the emulsifying device 2. The transfer device 3 is in communication with both the mixing device 1 and the reaction device 4 such that the transfer device 3 is capable of delivering the mixture from the mixing device 1 to the reaction device 4 for reaction with thionyl chloride in the reaction device 4 to produce dichlorosulfimide. Thus, the system for preparing bischlorosulfonimide according to the first embodiment of the present application can realize batch reaction.

In this embodiment, as shown in fig. 1, the mixing apparatus 1 includes a mixing tank 11, a dispersing agitator 12, and an agitator motor 13, and the mixing tank 11 includes a first inlet and a first outlet and is configured to receive and contain sulfamic acid and chlorosulfonic acid. The working condition of the mixing kettle 11 is normal temperature and normal pressure, and the energy consumption is low. The dispersing stirrer 12 is arranged in the mixing kettle 11 and is in transmission connection with a stirrer motor 13 positioned outside the mixing kettle 11. In a state where the agitator motor 13 is energized, the rotor of the agitator motor 13 can drive the dispersing agitator 12 so that the dispersing agitator 12 can agitate the mixture of sulfamic acid and chlorosulfonic acid in the mixing tank 11 with an agitating speed (rotational speed) of 200rpm to 500rpm (where rpm means revolutions per minute) for 0.5h to 1h (where h means hours). In this way, the stirring speed (rotation speed) and the shear line speed of the liquid-solid two phases (sulfamic acid and chlorosulfonic acid) in the mixing tank 11 can be increased, the collisions and disturbance between the two materials, between the materials and the dispersing stirrer 12, and between the materials and the walls of the mixing tank 11 can be enhanced, and the mixture can be easily formed into a slurry in which the two materials are uniformly dispersed.

In this embodiment, as shown in fig. 1, the emulsifying device 2 includes a second inlet connected to the first outlet of the mixing tank 11 of the mixing device 1 and a second outlet connected to the second outlet of the mixing tank 11 of the mixing device 1. Whereby both the second inlet and the second outlet of the emulsifying device 2 are in communication with the mixing device 1, so that the mixture from the mixing device 1 can be cyclically emulsified via 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 in communication with a first outlet of the mixing tank 11 at the bottom and the outlet is in communication with a first inlet of the mixing tank 11 at the top, the emulsifying pump 21 being capable of pumping slurry from the bottom of the mixing tank 11 of the mixing device 1. The emulsification motor 22 is a variable frequency motor, and the emulsification motor 22 is in transmission connection with the emulsification pump 21. In the state that the emulsification motor 22 is electrified, the rotor of the emulsification motor 22 drives the rotor of the emulsification pump 21 to rotate at a high speed, so that shearing, extrusion, collision and crushing of raw materials are realized by utilizing the rotor of the emulsification pump 21, the mixing uniformity of the raw materials is enhanced, the emulsification pump 21 is used for carrying out emulsification operation on mixed slurry to further improve the mixing uniformity of the raw materials, and then one raw material is uniformly dispersed in the other raw material in the form of very small particles/liquid drops, so that slurry with better uniformity is obtained. The slurry in the mixing device 1 may be emulsified by the emulsifying device 2 in a plurality of cycles (for example, 3 to 4 times), and the number of cycles may be adjusted as needed.

In this embodiment, as shown in fig. 1, a material transferring device 3 is connected between a mixing device 1 and a reaction device 4. Specifically, the transfer device 3 is in direct communication with the mixing device 1 for transporting the mixture after emulsification in the mixing device 1 out. The material transferring device 3 comprises a material transferring device 31 and a material transferring motor 32. The diverter 31 may be a screw conveyor or other device with conveying function, with the inlet of the diverter 31 always communicating with the first outlet at the bottom of the mixing tank 11 and the outlet communicating with the reaction apparatus 4. The material transferring motor 32 is a variable frequency motor, and the material transferring motor 32 is in transmission connection with the material transferring device 31, so that the material transferring motor 32 can drive the material transferring device 31 to convey the mixture in the mixing kettle 11 to the reaction device 4. The material transferring device 3 is always communicated with the mixing device 1 without a control valve, the same function of opening and closing the control valve can be realized by utilizing the opening and closing of the material transferring motor 32, namely, the quantity of mixture (slurry) transportation is controlled, the reduction of the channel section of a pipeline or a pipeline caused by the adjustment of the control valve is avoided, and the risk that the pipeline or the pipeline of a system is blocked and further corrosion and safety problems are caused is reduced.

In this embodiment, as shown in fig. 1, the reaction apparatus 4 is in communication with the transfer apparatus 3, so that the transfer apparatus 3 can convey the mixture from the mixing apparatus 1 to the reaction apparatus 4 to chemically react with thionyl chloride in the reaction apparatus 4 to produce dichlorosulfimide. It will be appreciated that the reaction device 4 comprises a reaction vessel with adjustable reaction pressure, the inlet of which communicates with the outlet of the rotor 31 of the rotor 3. The reaction vessel may be any vessel capable of smoothly carrying out the above chemical reaction safely and smoothly, for example, a reaction vessel, a reactor, a generator, a synthesis column, etc.

In the present embodiment, as shown in fig. 1, the feeding device 5 communicates with the mixing device 1 via the metering device 6, so that sulfamic acid from the feeding device 5 is metered via the metering device 6 and then fed into the mixing device 1. The feeder 5 may be an automated feeder. The metering device 6 comprises a silo 61 and a weight sensor 62. The inlet of the bin 61 is communicated with the feeding device 5, and the outlet of the bin 61 is communicated with the mixing kettle 11 of the mixing device 1. A weight sensor 62 is mounted to the bin 61 and is used to sense the weight of sulfamic acid in solid form added to the bin 61. Thus, not only can the automatic feeding process be completed through the automatic feeding machine, but also the sulfamic acid after accurate metering can be conveyed into the mixing kettle 11 through the metering device 6, and further the operation process of the automatic feeding machine can be controlled through metering data fed back by the metering device 6.

Further, in the present embodiment, as shown in fig. 1, the preparation system includes a first flow sensor FC1 and a control valve V. The control valve V may be electrically or signally connected to the first flow sensor FC1 such that the control valve V is opened and closed based on a parameter detected by the first flow sensor FC1, the first flow sensor FC1 being adapted to sense the flow rate of the liquid-phase chlorosulfonic acid delivered into the mixing device 1. In this way, accurate feeding of chlorosulfonic acid can be achieved with such lockout control. It will be appreciated that electrical or signal connections may be made indirectly through the controller. The electrical or signal connections described herein may be implemented in the same manner and will not be repeated below.

Further, the preparation system also includes a second flow sensor FC2. The second flow sensor FC2 may be electrically or signally connected to the emulsifying motor 22 such that the emulsifying motor 22 is opened and closed based on a parameter detected by the second flow sensor FC2, the second flow sensor FC2 being for sensing the flow rate of the slurry flowing from the outlet of the emulsifying pump 21 to the mixing tank 11 of the mixing apparatus 1. In this way, an accurate control of the amount of slurry that has been emulsified can be achieved with this control.

Further, the preparation system further comprises a third flow sensor FC3. The third flow rate sensor FC3 may be electrically or signally connected to the transfer motor 32 such that the transfer motor 32 is opened and closed based on the parameter detected by the third flow rate sensor FC3, and the third flow rate sensor FC3 is configured to sense the flow rate of the mixture flowing from the outlet of the transfer device 31 to the reaction apparatus 4. In this way, accurate control of the amount of slurry fed into the reaction device 4 can be achieved with such control.

The following describes a system for producing bischlorosulfonimide according to the second embodiment of the present application.

(System for producing bischlorosulfonimide according to the second embodiment of the application)

As shown in fig. 2, the system for preparing bischlorosulfonimide according to the second embodiment of the present application comprises all devices and connecting lines of the system for preparing bischlorosulfonimide according to the first embodiment of the present application, and is provided with additional structure, and the differences between the two are mainly described below.

In the present embodiment, unlike the first embodiment, as shown in fig. 2, two identical sets of subsystems are provided corresponding to the same inverting apparatus 3, each subsystem including a mixing apparatus 1, an emulsifying apparatus 2, a metering apparatus 6, and a feeding apparatus 5, and sensors and control valves corresponding to these apparatuses. The two subsystems are independent of each other and are connected in parallel with each other in the preparation system. Moreover, in each set of subsystems, the mixing device 1 and the emulsifying device 2 are arranged in groups in cooperation with each other, and the mixing devices 1 in both sets of subsystems are communicated with the same material transferring device 3. Further, a corresponding control valve (not shown) may be provided between the mixing device 1 and the transfer device 3 of each subsystem, so that it is possible to continuously feed the mixture (slurry) of sulfamic acid and chlorosulfonic acid into the reaction device 4 via the transfer device 3 by both subsystems, thereby enabling continuous feeding of the entire preparation system into the reaction device 4. In the case where the reaction apparatus 4 is used as a continuous reaction apparatus, the production system according to the present embodiment is capable of continuous reaction. It will be appreciated that in other alternatives, the mixing devices 1 of the two sets of subsystems may also be in communication with different transfer devices 3, respectively, where the different transfer devices 3 are all connected to the same reaction device 4.

It should be understood that the above-described embodiments are merely exemplary and are not intended to limit the present application. Those skilled in the art can make various modifications and changes to the above-described embodiments without departing from the scope of the present application. Further, the following supplementary explanation is made.

I. In a variant of the above second embodiment, more sets of subsystems in parallel with each other may be provided to enable continuous feeding of sufficient raw material.

In the modification of the above first and second embodiments, the on-line dispersing device may be used instead of the emulsifying device 2 as the homogenizing device, and the same technical effects can be achieved.

It will be appreciated that in a variant of the above first embodiment, only one of the dosing device 5 and the metering device 6 may be provided. In the case of a feed device 5 alone, the feed device 5 can be in direct communication with the mixing device 1 for feeding sulfamic acid into the mixing device 1, in which case sulfamic acid in the feed device 5 can be metered in by means of a metering device external to the preparation system. In the case of only the metering device 6, the metering device 6 can be in direct communication with the mixing device 1, and the sulfamic acid conveyed is metered by the metering device 6 and then conveyed into the mixing device 1, wherein the metering device simultaneously plays a role in metering and feeding.

In the preparation system of the dichlor sulfimide, a dispersing and emulsifying process is adopted, and a high-efficiency dispersing stirrer 12 in a mixing device 1 and a matched external circulation emulsifying device 2 are utilized to rapidly and uniformly disperse solid and liquid two-phase raw materials (sulfamic acid and chlorosulfonic acid). In addition, the particle size of the solid raw material is reduced, and particularly, the particle size can be reduced to a micron level (for example, the particle size is 40-80 microns), so that the surface area of the liquid-solid raw material reaction is increased, the reaction conversion rate is improved, and the production efficiency of the bischlorosulfimide is improved. In addition, after the slurry passes through the dispersion and emulsification system, the uniformity is obviously improved, the problem of particle agglomeration and blockage caused by solid accumulation or liquid phase encapsulation does not occur in the preparation system, the local overheating phenomenon caused by uneven heat transfer does not occur, and the possibility of potential safety hazard is reduced.

Claims (10)

1. A system for preparing a bis-chlorosulfonyl imide comprising:

Mixing means 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, the second inlet being connected to the first outlet, the second outlet being connected to the first inlet, the mixture in the mixing device being cyclically emulsified or cyclically dispersed by the homogenizing device, and

And the reaction device is communicated with the mixing device and receives the mixture, and the mixture and thionyl chloride react in the reaction device to generate dichloro-sulfonyl imide.

2. The system for preparing bischlorosulfonimide according to claim 1, wherein,

Further comprises a metering device which is communicated with the mixing device to meter the conveyed sulfamic acid and/or,

The mixing device is communicated with the mixing device, and the mixing device is used for conveying sulfamic acid into the mixing device.

3. The system for preparing a bischlorosulfonimide according to claim 2, wherein said metering device comprises a silo and a weight sensor, said silo outlet being in communication with said mixing device, said weight sensor being mounted to said silo and being adapted to sense the weight of sulfamic acid added to said silo.

4. The system for producing bis-chlorosulfonimide according to claim 1, further comprising a first flow sensor for sensing the flow rate of chlorosulfonic acid fed into the mixing device and a control valve that opens and closes based on a parameter detected by the first flow sensor.

5. The system for producing bischlorosulfonimide according to any of claims 1 to 4, wherein said homogenizing device comprises an emulsifying pump and an emulsifying motor, wherein the inlet of said emulsifying pump is in communication with the first outlet of said mixing device and the outlet is in communication with the first inlet of said mixing device, and wherein said emulsifying motor is in driving connection with said emulsifying pump, or

The homogenizing device comprises an on-line dispersing device.

6. The system for producing a bischlorosulfonimide according to claim 5, further comprising a second flow sensor, wherein said emulsifying motor is opened and closed based on a parameter detected by said second flow sensor, said second flow sensor being for sensing a flow rate of a mixture flowing from an outlet of said emulsifying pump to said mixing device.

7. The system for producing a bischlorosulfonimide according to any of claims 1 to 4, wherein said mixing device comprises a mixing kettle for containing sulfamic acid and chlorosulfonic acid, a dispersing agitator in driving connection with said agitator motor, and/or,

The stirring speed of the mixing device is 200rpm to 500rpm.

8. The system for producing a bischlorosulfonimide according to any of claims 1 to 4, further comprising a transfer device connected between said mixing device and said reaction device,

The material transferring device comprises a material transferring device and a material transferring motor, wherein an inlet of the material transferring device is communicated with a first outlet of the mixing device, an outlet of the material transferring device is communicated with the reaction device, and the material transferring motor is in transmission connection with the material transferring device.

9. The system for producing a bischlorosulfonimide according to claim 8, further comprising a third flow sensor for sensing a flow rate of the mixture flowing from an outlet of said material converter to said reaction apparatus, and/or wherein said material converting motor is opened and closed based on a parameter detected by said third flow sensor

The first outlet of the mixing device is always communicated with the material converter.

10. The system for producing bischlorosulfonimide according to any of claims 1 to 4, wherein said mixing means and said homogenizing means are arranged in groups and at least two groups are arranged in parallel to each other.