CN117361453A

CN117361453A - Method and device for continuously preparing high-purity dichloro sulfonyl imide acid

Info

Publication number: CN117361453A
Application number: CN202311126376.2A
Authority: CN
Inventors: 黄福亮; 郭剑煌; 林涌; 肖钦荣; 刘文通
Original assignee: Fujian Dexu New Material Co ltd
Current assignee: Fujian Dexu New Material Co ltd
Priority date: 2023-09-01
Filing date: 2023-09-01
Publication date: 2024-01-09
Anticipated expiration: 2043-09-01
Also published as: CN117361453B

Abstract

The invention relates to a method and a device for continuously preparing high-purity dichloro sulfonyl imide acid, which comprises the following steps: s1, mixing chlorosulfonyl isocyanate and chlorosulfonic acid in a mass-volume ratio of 4 kg-4.5 kg to 1L in a nitrogen environment; s2, heating a mixture of chlorosulfonyl isocyanate and chlorosulfonic acid to obtain a bischlorosulfonyliminoacid reaction solution; and S3, rectifying and purifying the reaction liquid of the dichloro sulfimide acid to obtain the high-purity dichloro sulfimide acid.

Description

Method and device for continuously preparing high-purity dichloro sulfonyl imide acid

Technical Field

The invention relates to the field of dichloro sulfonyl imide acid, in particular to a method and a device for continuously preparing high-purity dichloro sulfonyl imide acid.

Background

Along with the basic research and application of the power lithium ion battery, the lithium bis (fluorosulfonyl) imide becomes one of research hotspots of international chemistry, and becomes a novel lithium salt with the fastest industrialization progress due to excellent structural stability and electrochemical performance. The lithium bis (fluorosulfonyl) imide can not only improve the conductivity and safety of the lithium ion battery, but also remarkably improve the high-low temperature performance of the lithium ion battery. The dichloro-sulphonyl-imine acid is used as an important intermediate for synthesizing the difluoro-sulphonyl-imine lithium.

In the prior art, the method of adopting the tubular reactor to prepare the dichloro sulfonyl imide acid reaction solution can shorten the process line through the tubular reactor, thereby achieving the purposes of continuous production and improvement of production efficiency, but in the existing tubular reactor, the method of natural reaction is often adopted, or the method of directly adopting the heating of reactants is adopted, the whole reaction process is heated unevenly, the reaction cannot completely reach the reaction condition, and the purity and the yield of the product are greatly influenced.

After the dichloro sulfinamide acid reaction solution is prepared, the dichloro sulfinamide acid reaction solution is subjected to rectification treatment in a rectification tower, and the dichloro sulfinamide acid product is obtained by rectification. The reaction liquid of the dichlorsulfoimide acid contains unreacted chlorosulfonyl isocyanate and chlorosulfonic acid, the boiling point of the chlorosulfonyl isocyanate is 107 ℃, the boiling point of the dichlorsulfoimide acid is 115 ℃, the boiling points of the two are very close, and the boiling point of the chlorosulfonic acid is 151 ℃, and the difference between the boiling point of the dichlorsulfoimide acid and the boiling point of the dichlorsulfoimide acid of the chlorosulfonyl isocyanate is far. Therefore, the reboiler of the rectifying tower needs to be controlled to be higher than 151 ℃ to vaporize chlorosulfonic acid; the chlorosulfonyl isocyanate and the bischlorosulfonylimide acid have easy fluidity, the chlorosulfonic acid has semi-oiliness, the chlorosulfonic acid is easy to be adhered on the surface of the packing layer in the rectifying tower so as to block the packing layer, the chlorosulfonic acid is more difficult to flow downwards, and the chlorosulfonyl isocyanate and the bischlorosulfonylimide acid are easy to flow downwards like water, so that the chlorosulfonyl isocyanate and the bischlorosulfonylimide acid are easy to cover the outer surface of the chlorosulfonic acid, and the chlorosulfonic acid is not easy to participate in heat exchange to form liquid or gas.

The invention aims at the problems existing in the prior art by designing a method and a device for continuously preparing high-purity dichloro sulfonyl imide acid.

Disclosure of Invention

The present invention is directed to a method and apparatus for continuously preparing high-purity bis-chlorosulfonyl imide acid, which can effectively solve at least one of the problems of the prior art.

The technical scheme of the invention is as follows:

a method for continuously preparing high-purity dichlorosulfonyliminoacid, comprising the steps of:

s1, mixing chlorosulfonyl isocyanate and chlorosulfonic acid in a mass-volume ratio of 4 kg-4.5 kg to 1L in a nitrogen environment;

s2, heating a mixture of chlorosulfonyl isocyanate and chlorosulfonic acid to obtain a bischlorosulfonyliminoacid reaction solution;

and S3, rectifying and purifying the reaction liquid of the dichloro sulfimide acid to obtain the high-purity dichloro sulfimide acid.

Further, in step S2, heating the chlorosulfonyl isocyanate and chlorosulfonic acid mixture includes: the chlorosulfonyl isocyanate and chlorosulfonic acid mixture is fed into a tubular reactor at a flow rate of 2-5 kg/min, and the tubular reactor is used for heating the chlorosulfonyl isocyanate and chlorosulfonic acid mixture to 90-150 ℃.

Further, in step S3, the rectification and purification of the reaction solution of the bischlorosulfinic acid comprises: purifying the dichloro sulfinamide acid reaction solution in a rectifying tower, wherein the negative pressure operation is carried out in the rectifying tower, and the temperature of the top of the rectifying tower is set to be 110-120 ℃.

Further provided is an apparatus for continuously preparing high-purity dichlorosulfonyliminoacid, comprising:

two raw material tanks for storing chlorosulfonyl isocyanate and chlorosulfonic acid respectively;

the mixing tank is used for receiving chlorosulfonyl isocyanate and chlorosulfonic acid output by the two raw material tanks, and is used for providing a nitrogen environment and storing chlorosulfonyl isocyanate and chlorosulfonic acid mixed solution;

a high-pressure plunger pump for outputting the mixed liquid in the mixing tank;

the tubular reactor is used for receiving the mixed liquid output by the high-pressure plunger pump, enabling the mixed liquid to flow through at a constant speed and heating the mixed liquid, and enabling the mixed liquid to uniformly react to generate dichloro-sulfonyl imide acid reaction liquid;

and the rectifying tower is connected to the tubular reactor and is used for receiving the dichloro sulfinamide acid reaction solution and rectifying and purifying the dichloro sulfinamide acid reaction solution to obtain high-purity dichloro sulfinamide acid.

Further, the tubular reactor includes:

the inner tube part is provided with a plurality of linear cavity tubes and a plurality of arc cavity tubes, the linear cavity tubes and the arc cavity tubes are alternately connected, and flange plate seats are welded at two ends of the linear cavity tubes and the arc cavity tubes;

the outer tube part comprises a transverse circulating tube nested on the outer peripheral surface of the linear cavity tube and a lateral circulating tube nested on the outer peripheral surface of the arc cavity tube;

the steam circulation structure comprises a communicating pipe connected with an external steam source, a transverse flow pipe communicated with the communicating pipe, a plurality of transverse matching pieces which are arranged below the transverse flow pipe and are inserted into all the transverse circulation pipes, a plurality of longitudinal flow pipes which are vertically and fixedly connected to the transverse flow pipe and are flush with the transverse flow pipe, a plurality of longitudinal matching pieces which are arranged below the longitudinal flow pipe and are inserted into the lateral circulation pipes, and the shape and the structure of the transverse matching pieces are the same as those of the longitudinal matching pieces.

Further, the back mixing structure is installed at both axial ends of the inside of the linear cavity tube, the back mixing structure comprises a positioning plate installed in the linear cavity tube, a hanging seat fixed in the positioning plate, a spring locked on the hanging seat, a pushing ball installed on the spring, and a clamping cylinder for supporting the pushing ball.

Further, the rectifying column includes:

the tower body, the tower body top is provided with the steam outlet, the tower body bottom is provided with the liquid outlet, the tower body is close to the position of top and is provided with first inlet, the tower body is close to the position of bottom and is provided with the second inlet, the position in the middle of the tower body is provided with the third inlet, the tower body bottom is provided with the liquid outlet; the tower body is provided with a rotating device, the rotating device comprises a rotating motor arranged at the top end of the tower body, a rotating shaft arranged in the tower body, and a plurality of rotating paddles arranged in parallel on the rotating shaft, the rotating shaft is driven by the rotating motor, and the rotating shaft can be driven up and down so as to drive the rotating paddles to move up and down; the tower body is internally provided with a packing layer placing frame capable of moving up and down in a hanging manner above each rotating paddle, a packing layer is placed in the packing layer placing frame, the bottom of the packing layer placing frame is provided with a plurality of backflow holes for backflow liquid to flow downwards, the middle of the packing layer placing frame is provided with a through hole for enabling a rotating shaft to pass through, the rotating paddles can be lifted up after moving upwards to enable the packing layer placing frame to drive the packing layer placing frame to rotate together, and the rotating paddles can be separated from the bottom surface of the packing layer placing frame after moving downwards so that the packing layer placing frame is hung in the tower body and does not rotate.

The condenser is connected to the steam outlet and is used for condensing the gas-phase material flow at the top end of the tower body to form reflux liquid;

the reflux tank is connected between the condenser and the first liquid inlet and is used for storing and refluxing the reflux liquid;

and the reboiler is connected between the liquid outlet and the second liquid inlet and is used for heating and vaporizing the liquid at the bottom end of the tower body.

Further, the bottom surface of the packing layer placement frame is provided with a plurality of radial elastic sheets which are connected in a single end and are opened downwards, the elastic sheets enable the bottom surface of the packing layer placement frame to present a plurality of openings, the size of each opening is configured to prevent the packing layer from falling down, the bottom surface of the packing layer placement frame is fixedly provided with a connecting block on the outer ring of the elastic sheet, the connecting block protrudes out of the bottom surface of the packing layer placement frame, and the protruding height of the connecting block is smaller than the height of the tail end of each opening;

when the rotating paddles move upwards to a position which can touch one end of the elastic piece, which is not connected with the filler layer placing frame, and cannot contact the connecting block, the rotating paddles enable the elastic piece to regularly swing towards the bottom surface of the filler layer placing frame, so that the filler layer in the filler layer placing frame is driven to regularly vibrate;

When the rotating paddles move upwards to a position capable of supporting the packing layer placement frame, the rotating paddles swing upwards to close the opening through the elastic pieces, the rotating paddles can contact the connecting block, and the rotating paddles are clamped with the connecting block to drive the packing layer placement frame to rotate.

Further, the output shaft of the rotating motor and the rotating shaft are in sleeved connection through a connecting seat in a sliding manner, a screw rod assembly is arranged between the output shaft of the rotating motor and the rotating shaft and comprises a screw rod motor, a screw rod and a screw rod nut, the screw rod nut is fixedly connected with the connecting seat, the screw rod motor is fixedly arranged on the rotating shaft, the screw rod motor drives the screw rod nut to move up and down through the screw rod, so that the connecting seat is driven to move up and down, and the traction piece is hinged between the connecting seat and the baffle.

Further, the control method of the rectifying tower comprises the following steps:

a1, receiving the dichloro-sulfonyl imide acid reaction liquid from the third liquid inlet, controlling the reboiler to heat and vaporize the dichloro-sulfonyl imide acid reaction liquid at the bottom end of the tower body, controlling the condenser to condense a gas-phase material flow at the top end of the tower body to form reflux liquid, and enabling the reflux liquid to enter the tower body from the first liquid inlet;

The following steps are circularly executed until the purity of the dichlorsulfoximine acid at the bottom end of the tower body meets the preset requirement:

a2, driving the rotating paddles to move downwards, enabling the rotating paddles to be separated from the bottom surface of the packing layer placing frame, enabling the packing layer placing frame to be hung in the tower body, and entering the next step after keeping the first time;

a3, driving the rotating paddles to move upwards to a position which can touch one end of the elastic sheet, which is not connected with the filler layer placing frame, and cannot contact with the connecting block, driving the rotating paddles to rotate through the rotating motor, enabling the rotating paddles to rotate so as to drive the elastic sheet to regularly swing towards the bottom surface of the filler layer placing frame, further driving the filler layer in the filler layer placing frame to regularly vibrate, shaking off a part of chlorosulfonyl isocyanate and dichlorsulfonylimide acid attached to the filler layer, and entering the next step after keeping for a second time;

a4, driving the rotating paddles to move upwards to a position capable of supporting the packing layer placing frame, enabling the rotating paddles to support the packing layer placing frame so as to drive the packing layer placing frame to rotate together, enabling the packing layer to fully contact with rising gas with backflow liquid, and entering the next step after maintaining for a third time;

A5, enabling the rotating paddles to support the packing layer placing frame so as to drive the packing layer placing frame to rotate together, enabling chlorosulfonic acid attached to the packing layer to be centrifugally thrown out and flow downwards, and returning to the step A2 after the fourth time is kept.

Accordingly, the present invention provides the following effects and/or advantages:

the invention overcomes the defects of complex reaction, more three wastes, high equipment requirement, relatively low yield and high energy consumption in the prior art, and aims to break the technical barrier, the developed preparation method and device have the advantages of simple raw material components, short process line, continuous production and improved production efficiency and product yield, thereby realizing the high-efficiency and high-purity industrial production of the bischlorosulfinamic acid.

The method and the device can obtain the high-purity dichloro sulfonyl imide acid with the purity of 99.5 percent under the conditions of simple reaction raw materials and simple reaction device; the method and the device can realize continuous production, improve the production efficiency, reduce the production energy consumption and shorten the production period; the method has the advantages of simple raw materials and few by-product three wastes, can effectively reduce the energy consumption for separation and purification and simultaneously responds to the call of national energy-saving chemical industry and clean chemical industry; the method has relatively simple reaction raw materials and reaction devices, and is more beneficial to the industrial production of the dichloro sulfonyl imide acid.

By the device and the control method provided by the application, the purity and the molar yield of the dichlorsulfamic acid can be improved.

According to the device, when the rotating slurry drives the packing layer placing frame to rotate, on one hand, the packing layer in the packing layer placing frame can be driven to rotate, so that contact between gas-phase logistics and reflux liquid is realized rapidly; on the other hand, the packing layer placing frame generates centrifugal force, and when rotating at a low speed, part of reflux liquid can be thrown out so as to separate from the packing layer, so that dichlorosulfonyliminoic acid and chlorosulfonyl isocyanate in the reflux liquid are separated from the surface of the separating packing layer, chlorosulfonic acid on the surface of the packing layer is exposed, chlorosulfonic acid is contacted with gas-phase logistics, and when rotating at a high speed, the separation of dichlorosulfonyliminoic acid and chlorosulfonyl isocyanate in the reflux liquid from the surface of the separating packing layer can be realized, and chlorosulfonic acid can be separated from the separation of the surface of the packing layer under the action of larger centrifugal force, so that the reflux liquid in a downflow state is rapidly formed from the bottom of the packing layer placing frame. Therefore, the heat exchange efficiency can be improved, and the purification effect of the dichlorsulfoximine acid can be improved.

The control method corresponding to the device provided by the application comprises the following operation of circulation: the packing layer placing frame is kept motionless, the elastic sheet is touched, the packing layer placing frame rotates at a low speed, the packing layer placing frame rotates at a high speed, so that reflux liquid is accumulated on the packing layer in the step A2, other components covered on the outer surface of chlorosulfonic acid on the surface of the packing layer are dropped through vibration of the elastic sheet in the step A3, gas phase and liquid phase are further contacted, the packing layer placing frame is driven to rotate at a low speed in the step A4, the gas phase and the liquid phase are driven to fully and rapidly contact, and finally the packing layer placing frame is driven to rotate at a high speed in the step A5, so that chlorosulfonic acid is centrifugally thrown out and flows downwards. The step performed by this cycle can sufficiently purify the bischlorosulfonyliminoacid.

The outside of the continuous tube type reactor of the device provided by the application is provided with the sleeve type structure of the transverse circulating tube and the lateral circulating tube, the steam circulating structure is connected into the sleeve type structure, and the continuous tube type reactor is internally kept with stable reaction temperature in a steam circulating mode, so that the reaction of the dichloro sulfimide acid can be promoted under the condition of a simple reactor, the temperature is stable in the reaction process, and the conversion rate of the product is high. The invention further provides a setting mode for dividing a steam circulation structure into a transverse circulation pipe and a longitudinal circulation pipe, and the transverse circulation pipe and the longitudinal circulation pipe are respectively inserted into the transverse circulation pipe and the lateral circulation pipe through a transverse matching piece and a longitudinal matching piece to respectively carry out independent steam heat circulation on the transverse circulation pipe and the lateral circulation pipe, so that each position in the continuous pipe reactor is in a constant temperature state, and the reaction can be continuously carried out.

It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to provide further explanation of the invention as claimed.

Drawings

Fig. 1 is a schematic flow chart of the method provided by the invention.

Fig. 2 is a schematic structural diagram of the device provided by the invention.

FIG. 3 is a schematic elevational view of the tubular reactor.

FIG. 4 is a schematic view showing the structure of the lateral installation structure of the tube reactor in cooperation with the lateral circulation tube.

Fig. 5 is a schematic side view of a side mounting structure of a tubular reactor.

FIG. 6 is a schematic left-hand structural view of a flange seat of a tubular reactor.

FIG. 7 is a schematic view of the structure of a transverse circulation pipe of a pipe reactor.

Fig. 8 is a schematic structural view of a lateral circulation tube of a tubular reactor (disassembled state).

Fig. 9 is a schematic front view of the steam cycle structure of the tubular reactor.

FIG. 10 is a schematic structural view of a lateral fitting of a tubular reactor.

FIG. 11 is a schematic structural view of a back-mixing structure of a tubular reactor.

Fig. 12 is a schematic structural diagram of the rectifying column.

Fig. 13 is a schematic view of the structure of the packing layer placement frame and the rotary slurry.

Fig. 14 is a schematic diagram showing the structure of the two cross sections of the shaft after explosion of the packing layer placement frame and the rotary slurry.

Fig. 15 is a schematic structural view of the rotating device.

Fig. 16 is a schematic structural view of the screw assembly.

Fig. 17 is a schematic bottom view of the packing layer placement frame and the packing layer placement frame after the explosion of the rotating paddles (the reflow holes are hidden in fig. 17 for ease of illustration).

Detailed Description

For the convenience of understanding by those skilled in the art, the structure of the present invention will now be described in further detail with reference to the accompanying drawings:

referring to fig. 1, a method for continuously preparing high-purity dichlorosulfonylimide acid includes the steps of:

A method for continuously preparing high-purity dichlorosulfonyliminoacid can be represented by the following chemical reaction scheme:

among them, the prior art is that the sulfonyl isocyanate and chlorosulfonic acid react to form dichlorosulfonyliminoic acid, and the preparation method is disclosed in patent application number CN 202110373932.0. The preparation method has the defect that the purity of the prepared dichloro sulfonyl imide acid is low.

In the embodiment, chlorosulfonyl isocyanate and chlorosulfonic acid are respectively placed in a raw material tank according to the mass volume ratio of 4 kg-4.5 kg:1L; before the reaction, replacing air of all containers in the mixing tank with nitrogen through a nitrogen replacement device, and pumping raw materials into the mixing tank through a high-pressure plunger pump to perform primary mixing reaction; the mixed solution is pumped into a high-efficiency steam jacket tubular reactor by a high-pressure plunger pump at the flow rate of between 2 and 5kg/min under the condition that the flow rate is between 1.0 and 1.5Mpa, the mixed solution continuously passes through the tubular reactor at the same flow rate, the temperature is controlled between 90 and 150 ℃ to obtain a dichloro-sulfonylimide acid reaction solution, the dichloro-sulfonylimide acid reaction solution is input into a rectifying tower for rectification treatment, polytetrafluoroethylene filler is adopted as filler in the rectifying tower, the temperature resistance is up to 180 ℃, the total length of the filler at two ends is controlled between 2 and 3 m, and the filler layer has the advantages of larger specific surface area, high mass transfer efficiency, small flow resistance and the like and is fed at the middle-upper position; operating the rectifying tower at the negative pressure, wherein the temperature of the top of the rectifying tower is 110-120 ℃; the gas phase at the top of the tower enters a secondary condenser to be condensed, then enters a reflux tank to be pressurized by a reflux pump, and part of the gas phase returns to the raw material tank to reflux, and the other part of the gas phase is treated by waste. The heavy components at the bottom of the tower are sent to a product tank through a silicon carbide (SiC) reboiler. Finally, the high-purity dichloro sulfonyl imide acid is obtained at the bottom of the rectifying tower.

two raw material tanks 1 for storing chlorosulfonyl isocyanate and chlorosulfonic acid, respectively;

a mixing tank 2 for receiving chlorosulfonyl isocyanate and chlorosulfonic acid outputted from the two raw material tanks 1, and the mixing tank 2 for providing a nitrogen atmosphere and storing a chlorosulfonyl isocyanate and chlorosulfonic acid mixed solution;

a high-pressure plunger pump 5 for outputting the mixed liquid in the mixing tank 2;

the tubular reactor 3 is used for receiving the mixed solution output by the high-pressure plunger pump 5, enabling the mixed solution to flow through at a constant speed and heating the mixed solution, and enabling the mixed solution to uniformly react to generate a dichloro-sulfonyl imide acid reaction solution;

and the rectifying tower 4 is connected to the tubular reactor 3 and is used for receiving the dichloro sulfinamide acid reaction solution and rectifying and purifying the dichloro sulfinamide acid reaction solution to obtain high-purity dichloro sulfinamide acid.

Referring to fig. 3 to 11, the tubular reactor 3 includes: the inner pipe part 310, the inner pipe part 310 is provided with a plurality of linear cavity pipes 311 and a plurality of arc cavity pipes 312, the linear cavity pipes 311 and the arc cavity pipes 312 are alternately connected and arranged, and flange plate seats 313 are welded at two ends of the linear cavity pipes 311 and the arc cavity pipes 312; an outer tube part 320, wherein the outer tube part 320 comprises a transverse circulating tube 321 nested on the outer peripheral surface of the linear cavity tube 311 and a lateral circulating tube 322 nested on the outer peripheral surface of the arc-shaped cavity tube 312; the steam circulation structure 330, the steam circulation structure 330 includes a communicating pipe 331 connected to an external steam source, a lateral flow pipe 332 connected to the communicating pipe 331, a plurality of lateral matching members 333 disposed below the lateral flow pipe 332 and inserted into all the lateral circulation pipes 321, a plurality of longitudinal flow pipes 334 vertically fixedly connected to the lateral flow pipe 332 and flush with the lateral flow pipe 332, and a plurality of longitudinal matching members disposed below the longitudinal flow pipe 334 and inserted into the lateral circulation pipes 322, wherein the shape and structure of the lateral matching members 333 are the same as those of the longitudinal matching members.

In the reaction process, chlorosulfonyl isocyanate and chlorosulfonic acid are pumped into a mixing tank 2 by a high-pressure plunger pump according to the mass volume ratio of 4 kg-4.5 kg:1L for preliminary mixing reaction, and then the mixed solution is pumped into a tubular reactor in the embodiment, wherein the mixed solution directly reacts in a tubular reactor 3 which is arranged in a winding way, gradually passes through a straight-line cavity tube 311 and an arc-shaped cavity tube 312 which are alternately arranged, and the straight-line cavity tube 311 and the arc-shaped cavity tube 312 are connected by a flange seat 313.

In this embodiment, in the preparation process of the bischlorosulfonyliminoacid, the problems of more reaction waste, low yield and high energy consumption are difficult to solve, the preparation process with high cost is always an industry pain point, in the invention, the continuous tubular reactor formed by the linear cavity tube 311 and the arc cavity tube 312 is adopted first, the reactants can be connected and reacted in the long-distance tubular reactor, the sleeve type structure of the transverse circulating tube 321 and the lateral circulating tube 322 is constructed outside the continuous tubular reactor, the steam circulating structure 330 is connected into the sleeve type structure, and the stable reaction temperature is kept in the continuous tubular reactor in a steam circulating manner, so that the reaction of the bischlorosulfonyliminoacid can be promoted under the condition of a simple reactor, the temperature is stable in the reaction process, and the product conversion rate is high.

In fact, the straight-line chamber tube 311 and the arc-shaped chamber tube 312 are designed separately, and although the interiors thereof are in a communicating state, the transverse circulating tube 321 and the lateral circulating tube 322 are not in communication due to the obstruction of the flange plate seat 313, and in this way, the invention further proposes a mode of dividing the steam circulating structure 330 into a transverse circulating tube 332 and a longitudinal circulating tube 334, and the transverse circulating tube 332 and the longitudinal circulating tube 334 are respectively connected to the transverse circulating tube 21 and the lateral circulating tube 322 by inserting the transverse matching piece 333 and the longitudinal matching piece, so that the independent steam heat circulation is respectively carried out on the transverse circulating tube 321 and the lateral circulating tube 322, thereby ensuring that each position in the continuous tubular reactor is in a constant temperature state, and the reaction can be continuously carried out.

The method of adding the steam sleeve pipe is beneficial to the whole reaction, but the pipeline of the inner pipe portion 310 is also isolated from the external environment directly, once the inner pipe portion 310 is leaked, the inner pipe portion 310 is difficult to overhaul, workers are difficult to directly cross the outer pipe portion 320 and the steam circulation structure 330 to test the inner pipe portion 310, the maintenance difficulty is improved, compared with the maintenance difficulty, the overhaul difficulty of the linear cavity pipe 311 positioned at the inner side position of the whole continuous pipe reactor is larger, even if the drilling overhaul is carried out in a narrow space, the refilling is extremely difficult, the transverse circulating pipe 321 comprises two semicircular pipes 3211 which are combined to form a circular pipe, the two semicircular rings 3213 connected at the top of the semicircular pipes 3211 are connected, the two semicircular rings 3211 and the sealing rubber strips 3214 of the inner side walls of the semicircular rings 3213 are glued, the two semicircular rings 3211 are adhered to form a circular ring structure, the length of the semicircular rings 3211 is shorter than the length of the linear cavity pipe 311, and the two semicircular rings 3211 can be directly dismounted from the inner side positions of the linear cavity pipe 311 through the corresponding semicircular rings 321 to the two semicircular rings 311, and the two semicircular rings 3211 can be directly dismounted in the sealing rubber strips 3 in the inner side positions of the semicircular pipes 3211.

In the above-described setting process, although the lateral circulation pipe 321 is set in a detachable state, the entire one and both end positions thereof and the engagement with the lateral engagement member 333 are liable to leak, thereby letting steam escape, for which reason, at both end positions of the lateral circulation pipe 321: a lateral mounting structure 340 is clamped at two sides of the transverse circulating pipe 321, the lateral mounting structure 340 comprises a clamping power structure 341 locked on the outer peripheral surface of the transverse circulating pipe 321, a movable disc 342 fixedly connected with the clamping power structure 341 and movably attached to the transverse circulating pipe 321, a sealing ring connected at the inner side of the movable disc 342 and attached to the transverse circulating pipe 321, a clamping seat 343 welded on the movable disc 342 and attached to the flange seat 313, a lateral mounting structure 340 is adopted, namely, the lateral mounting structure 340 and the clamping seat 343 extend the length of the lateral circulating pipe 321 upwards through the movable disc 342, in a use state, the lateral mounting structure 340 can be matched with the flange seat 313 on the linear cavity tube 311, in a non-use state, the lateral mounting structure 340 adopts a retraction mode to be directly removed from the whole transverse circulating pipe 321, and then a semicircular tube 3211 in the transverse circulating pipe 321 is separated and can be removed;

And at the mating position of the transverse circulation tube 321 with the transverse mating member 333, in particular: the transverse matching member 333 includes a column head 3331 fixedly connected below the transverse flow tube 332, an outer matching tube 3332 attached to the outer side of the column head 3331 and welded below the transverse flow tube 332, an inner matching tube 3333 vertically fixed to the bottom of the column head 3331 and spaced from the outer matching tube 3332, the inner matching tube 3333 is inserted into a circular structure formed by two semicircular rings 3213, the outer matching tube 3332 is sleeved outside the circular structure formed by two semicircular rings 3213, the structural characteristics of the transverse matching member 333 are directly utilized, the double-layer fixation is firstly performed on the circular structure formed by two semicircular tubes 3211 on the transverse flow tube 321 by adopting the matching mode of the outer matching tube 3332 and the inner matching tube 3333, and furthermore, in the embodiment, an elastic steel sheet 3334 is also provided to be fixed on the inner side of the inner matching tube 3333, the elastic steel sheet 3334 is tightly clamped and attached to the outer side of a circular ring structure formed by the semicircular rings 3213 and attached to the inner wall of the outer matching cylinder 3332 after being ejected, the elastic steel sheet 3334 is wrapped by a gap between the inner matching cylinder 3333 and the circular ring structure by using the wrapping effect of the elastic steel sheet 3334 under the attaching effect of the elastic steel sheet 3334, so that steam is prevented from flowing out of the circular ring structure, wherein the elastic steel sheet 3334 is arranged in two sections, one section is always arranged on the inner side of the inner matching cylinder 3333, the other section can be folded, the inner matching cylinder 3333 can be clamped into the circular ring structure formed by the semicircular rings 3213 after being straightened in the installation stage, and after the inner matching cylinder 3333 is completely matched with the circular ring structure, the lower half section of the elastic steel sheet 3334 is exposed out of the circular ring structure and can be folded under the influence of elasticity of the elastic steel sheet 3334 and is directly attached to the outer side wall of the circular ring structure, so that the multi-section sealing effect is formed.

In summary, on the basis that the transverse circulating pipe 321 is detachably arranged, the lateral mounting structure 340 and the transverse matching piece 333 are matched and fixed, so that the steam can ensure good circulation, reduce energy consumption, and promote stable reaction.

If the lateral mounting structure 340 is directly matched with the conventional flange seat 313, air tightness is difficult to ensure in the matching process, for this purpose, the back mixing structure 314 is mounted at both axial ends of the inside of the linear cavity tube 311, the back mixing structure 314 comprises a positioning plate 3141 mounted in the linear cavity tube 311, a hanging seat 3142 fixed in the positioning plate 3141, a spring 3143 locked on the hanging seat 3142, a pushing ball 3144 mounted on the spring 3143, and a clamping cylinder 3145 for supporting the pushing ball 3144, and a clamping disc 3133 and a closing ring 3134 are arranged on the flange seat 313, so that in the pushing process of the clamping seat 343 on the lateral mounting structure 340, the clamping disc 3133 is directly matched with the closing ring 3134, and meanwhile, the outside of the back mixing structure is limited by the closing ring 3134, so that the matching edge is sealed, the effect of the sealing is achieved, the steam is avoided, and the energy circulation is not lost.

It should be emphasized that the direction of movement of the push ball 3144 is always towards the end of the reactant so that back mixing is avoided rather than being impeded.

In addition, in order to make the pushing ball 3144 easier to be pushed up when being pushed by the reactant, the obstruction of the pushing ball 3144 to the reactant is reduced, an inclined surface is arranged on one side of the clamping cylinder 3145, which faces the pushing ball 3144, and the inclined surface is movably attached to the pushing ball 3144, so that the pushing ball 3144 can be facilitated to find a new blocking position again after being reset.

In the positioning plate 3141, a space through which the reactant passes is greatly compressed, and in order to facilitate the reactant to continuously move to the rear end, a plurality of holes 3146 are formed in the positioning plate 3141, and when the pushing ball 3144 is pushed away, the reactant passes through the holes 3146.

Referring to fig. 12 to 17, a rectifying column for purifying bischlorosulfinic acid, comprising:

the tower body 41, the top of the tower body 41 is provided with a steam outlet 411, the bottom of the tower body is provided with a liquid outlet, a first liquid inlet 412 is arranged at a position, close to the top, of the tower body 41, a second liquid inlet 413 is arranged at a position, close to the bottom, of the tower body 41, a third liquid inlet 414 is arranged at a position, in the middle of the tower body 41, and the bottom of the tower body 41 is provided with a liquid outlet 415;

A condenser 42 connected to the steam outlet 411 for condensing the gas phase stream at the top of the tower 41 to form a reflux;

a reflux drum 43 connected between the condenser 42 and the first liquid inlet 412 for storing and refluxing the reflux liquid;

a reboiler 44 connected between the liquid outlet 415 and the second liquid inlet, for heating and vaporizing the liquid at the bottom end of the tower 41;

in this embodiment, the principle of the rectifying tower is to continuously heat and evaporate the liquid at the bottom by using the reboiler 44 at the bottom, so that the liquid is evaporated and flows to the top of the tower. The condenser 42 condenses the vapor phase stream at the top of the column to form a reflux, which is returned to the top of the column from the first inlet 412, and the reflux flows downward from the top of the column. In the process of flowing down the reflux liquid, the reflux liquid is contacted with a gas phase stream generated by the reboiler 44, the gas phase stream exchanges energy with the reflux liquid, and part of energy in the gas phase stream is transferred to the reflux liquid, so that part of the reflux liquid is vaporized in the process of absorbing heat in the flowing down process, and part of the gas phase stream is liquefied in the rising process. The above-described process is repeated continuously, so that the light component and the low boiling point component in the liquid at the bottom of the column are separated to the top of the column and condensed and stored in the reflux drum 43, thereby achieving the purification effect. The structure and operation of the condenser 42, reflux drum 43, reboiler 44, and column 41 are straightforward in the prior art and will be described herein.

The tower body 41 is provided with a rotating device 45, the rotating device 45 comprises a rotating motor 451 arranged at the top end of the tower body 41, a rotating shaft 452 arranged in the tower body 41, and a plurality of rotating paddles 453 arranged in parallel on the rotating shaft 452, the rotating shaft 452 is driven by the rotating motor 451, and the rotating shaft 452 can be driven up and down so as to drive the plurality of rotating paddles 453 to move up and down;

the tower body 41 is internally provided with a packing layer placing frame 46 which can move up and down in a hanging manner above each rotating paddle 453, a packing layer 47 is placed in the packing layer placing frame 46, a plurality of reflux holes 461 for reflux downflow are formed in the bottom of the packing layer placing frame 46, through holes 462 for allowing the rotating shafts 452 to pass through are formed in the middle of the packing layer placing frame 46, the rotating paddles 453 can support the packing layer placing frame 46 after moving upwards so as to drive the packing layer placing frame 46 to rotate together, and the rotating paddles 453 can be separated from the bottom surface of the packing layer placing frame 46 after moving downwards so that the packing layer placing frame 46 is hung in the tower body 41 and does not rotate.

In this embodiment, the packing layer 47 is of a prior art, which may be of an irregular or regular, large surface area, large granular or corrugated configuration with a plurality of through holes or gaps, which function to provide a large surface area for the reflux to be dispersed as it passes through the packing layer 47, thereby providing a large surface area for the reflux to contact the vapor stream. The vapor stream may flow upward through return orifice 461 to contact the downward flowing return liquid. The filler layer 47 is prior art and is not deployed here.

Passive structures are used in the prior art for contacting a vapor stream with a reflux liquid. Since the present example is used for producing dichlorosulfonyliminoacid, the impurities contained in the reaction liquid of the dichlorosulfonyliminoacid are generally the raw materials remaining from the reaction, wherein the dichlorosulfonyliminoacid and chlorosulfonyl isocyanate are water-like liquids, the fluidity of the dichlorosulfonyliminoacid and chlorosulfonyl isocyanate is good, and the chlorosulfonic acid is semi-oily liquid, the fluidity of chlorosulfonic acid is inferior to that of chlorosulfonyl isocyanate or dichlorosulfonyliminoacid, and the chlorosulfonic acid easily adheres to the surface of the filler layer 47 when the chlorosulfonic acid flows through the filler layer 47, and the dichlorosulfonyliminoacid and chlorosulfonyl isocyanate more easily flow down along the surface of the filler layer 47 to which chlorosulfonic acid adheres. In addition, during the heat exchange of the return holes 461, the gas phase flow below is easier to open up the dichlorosulfonyliminoic acid and chlorosulfonyl isocyanate covered on the return holes 461, and the semi-oily characteristic of chlorosulfonic acid covered on the return holes 461 is easy to block the return holes 461. Thus, the efficiency of heat exchange is hindered by chlorosulfonic acid, and the desired product bischlorosulfonylimide acid mixed in chlorosulfonic acid is difficult to purify, which hinders the purification rate.

The core improvement of this embodiment is that a rotating device 45 is added for rotating the filler layer 47.

When the rotating slurry 453 does not drive the packing layer placing frame 46 to rotate, the packing layer placing frame 46 is naturally hung on the inner wall of the tower 41. In this state, the working principle of the embodiment is similar to that of the existing rectifying tower, and the process of naturally flowing down the reflux liquid and naturally flowing up the gas-phase material flow is adopted to passively contact, so that the heat exchange is completed, and the rectifying process is realized.

When the rotating slurry 453 drives the packing layer placement frame 46 to rotate, on one hand, the packing layer 47 in the packing layer placement frame 46 can be driven to rotate, so that contact between gas-phase logistics and reflux liquid is realized rapidly; on the other hand, the packing layer placing frame 46 generates centrifugal force, when rotating at a low speed, a part of reflux liquid can be thrown out so as to separate from the packing layer 47, so that the dichlorosulfonimide acid and chlorosulfonyl isocyanate in the reflux liquid are separated from the surface of the separation packing layer 47, chlorosulfonic acid on the surface of the packing layer 47 is exposed, the chlorosulfonic acid is contacted with gas-phase logistics, when rotating at a high speed, besides the separation of the dichlorosulfonimide acid and chlorosulfonyl isocyanate in the reflux liquid from the surface of the separation packing layer 47, the chlorosulfonic acid can be separated from the surface of the packing layer 47 under the action of larger centrifugal force, and thus, the reflux liquid in a downflow state can be rapidly formed to be downflow from the bottom of the packing layer placing frame 46. Therefore, the heat exchange efficiency can be improved, and the purification effect of the dichlorsulfoximine acid can be improved.

Further, a circle of clamping grooves 466 are formed in the side wall of the packing layer placement frame 46, a plurality of groups of clamping blocks 416 are arranged on the inner wall of the tower body, the packing layer placement frame 46 is hung in the tower body 41 through the clamping grooves 466 and the clamping blocks 416, and the thickness of the clamping blocks 416 is smaller than the width of the clamping grooves 466, so that the packing layer placement frame 46 can move up and down.

In this embodiment, the thickness of the clamping block 416 is smaller than the width of the clamping groove 466, so that the clamping groove 466 can be limited by the clamping block 416 to move up and down in a certain space. When the packing layer placing frame 46 is supported by the rotating slurry 453, the packing layer placing frame 46 can move along with the rotating slurry 453, and when the packing layer placing frame 46 is lowered by the rotating slurry 453, the packing layer placing frame 46 can be hung on the inner wall of the tower body 41 and does not rotate.

Referring to fig. 15 and 16, further, the output shaft of the rotating motor 451 and the rotating shaft 452 are slidably sleeved through a connecting seat 454, a screw rod assembly 48 is disposed between the output shaft of the rotating motor 451 and the rotating shaft 452, the screw rod assembly 48 includes a screw rod motor 481, a screw rod 482 and a screw rod nut 483, the screw rod nut 483 is fixedly connected with the connecting seat 454, the screw rod motor 481 is fixedly disposed on the rotating shaft 452, and the screw rod motor 481 drives the screw rod nut 483 to move up and down through the screw rod 482, so as to drive the connecting seat 454 to move up and down.

In this embodiment, the connecting seat 454 is fixedly connected with the rotating shaft 452, and the output shaft of the rotating motor 451 of the connecting seat 454 is slidably sleeved, so that the up-and-down movement of the connecting seat 454 can be controlled through the screw rod assembly 48, and the rotating shaft 452 is controlled to drive the rotating slurry 453 to move up and down. The lead screw motor 481 may be a stepping motor so that the displacement amount of the rotation shaft 452 can be controlled.

Further, a separation plate 417 is disposed at the top end of the tower 41, the separation plate 417 separates the top end of the tower 41 from a screw assembly installation cavity, and the screw assembly 48 is disposed in the screw assembly installation cavity.

Further, the steam outlet 411 communicates to the inside of the tower 41 through the partition plate 417.

Since the rotation motor 451 and the screw motor 481 cannot bear the high temperature of about 150 degrees celsius inside the rectifying tower, the embodiment isolates the high temperature inside the tower body 41 through the isolating plate 417, and the isolated screw assembly mounting cavity temperature is at the bottom, so that the screw motor 481 inside can conveniently work, and meanwhile, the heat transferred to the rotation motor 451 is reduced.

Further, the side wall of the packing layer placement frame 46 is provided with a plurality of rotating wheels 467.

The rotating wheel 467 can reduce the friction between the packing layer placing frame 46 and the inner wall of the tower 41 when the packing layer placing frame 46 rotates.

Example two

The first embodiment does not include the elastic sheet 464. The present embodiment adds the elastic sheet 464 to the first embodiment.

Referring to figures 13 and 14 (filler layer 47 is not shown in figures 13 and 14),

the bottom surface of the packing layer placement frame 46 is provided with a plurality of elastic pieces 464 which are radially and singly connected and downwards opened, the elastic pieces 464 enable the bottom surface of the packing layer placement frame 46 to present a plurality of openings, the sizes of the openings are configured not to enable the packing layer 47 to fall, the bottom surface of the packing layer placement frame 46 is fixedly provided with a connecting block 465 on the outer ring of the elastic pieces 464, the connecting block 465 protrudes out of the bottom surface of the packing layer placement frame 46, and the protruding height of the connecting block 465 is smaller than the height of the tail end of the opening;

when the rotating paddle 453 moves up to a position where the elastic piece 464 can touch the elastic piece 464 is not connected to one end of the packing layer placement frame 46 and cannot touch the connecting block 465, the rotating paddle 453 enables the elastic piece 464 to swing regularly towards the bottom surface of the packing layer placement frame 46, so as to drive the packing layer 47 in the packing layer placement frame 46 to vibrate regularly;

when the rotating paddle 453 moves upwards to a position capable of supporting the packing layer placement frame 46, the rotating paddle 453 swings the elastic piece 464 upwards to close the opening, the rotating paddle 453 can contact the connecting block 465, and the rotating paddle 453 is clamped with the connecting block 465 to drive the packing layer placement frame 46 to rotate.

The regular vibration of the filler layer 47 can primarily shake off the reflux liquid on the surface of part of the filler layer 47. This is because, if only the manner of rotating the packing layer placement frame 46 is adopted, the dichlorosulfonyliminoacid and chlorosulfonyl isocyanate in the reflux liquid are liable to separate from the packing layer 47 due to the strong fluidity characteristics of the dichlorosulfonyliminoacid and chlorosulfonyl isocyanate in the reflux liquid, which in turn results in a decrease in the contact area between the reflux liquid and the gas-phase stream, and a decrease in the heat exchange efficiency. By providing the elastic piece 464 and its positional relationship, in cooperation with the rotating paddle 453, heat exchange efficiency can be improved.

Further provided is a control method of a rectifying tower for purifying bischlorosulfinic acid, based on the rectifying tower for purifying bischlorosulfinic acid, the control method comprises the following steps:

a1, receiving the bischlorosulfonylimide acid reaction solution from the third liquid inlet 414, controlling the reboiler 44 to heat and vaporize the bischlorosulfonylimide acid reaction solution at the bottom end of the tower 41, controlling the condenser 42 to condense the gas phase stream at the top end of the tower 41 to form reflux liquid, and allowing the reflux liquid to enter the tower 41 from the first liquid inlet 412;

the following steps are cyclically executed until the purity of the dichlorosulfonylimide acid at the bottom end of the tower body 41 meets the preset requirement:

A2, driving the rotating paddles 453 to move downwards, enabling the rotating paddles 453 to separate from the bottom surface of the packing layer placing frame 46, enabling the packing layer placing frame 46 to be hung in the tower body 41, and entering the next step after keeping for the first time;

a3, driving the rotating paddle 453 to move upwards to a position which can touch one end of the elastic sheet 464 which is not connected with the packing layer placing frame 46 and cannot touch the connecting block 465, driving the rotating paddle 453 to rotate through the rotating motor 451, enabling the rotating paddle 453 to rotate to drive the elastic sheet 464 to regularly swing towards the bottom surface of the packing layer placing frame 46, further driving the packing layer 47 in the packing layer placing frame 46 to regularly vibrate, shaking off a part of chlorosulfonyl isocyanate and bischlorosulfonylimide acid attached to the packing layer 47, and keeping the second time and then entering the next step;

a4, driving the rotating paddle 453 to move upwards to a position capable of supporting the packing layer placing frame 46, enabling the rotating paddle 453 to support the packing layer placing frame 46 so as to drive the packing layer placing frame 46 to rotate together, enabling the packing layer 47 to fully contact with rising gas with backflow liquid, and keeping for a third time and then entering the next step;

A5, the rotating paddle 453 supports the packing layer placing frame 46 so as to drive the packing layer placing frame 46 to rotate together, so that chlorosulfonic acid attached to the packing layer 47 is centrifugally thrown out and flows downwards, and the step A2 is returned after the fourth time.

Further, in A4, the rotating paddle 453 is caused to lift the filler layer placement frame 46 so as to drive the filler layer placement frame 46 to rotate at a low speed.

Further, in A5, the rotating paddle 453 is caused to support the filler layer placement frame 46 so as to drive the filler layer placement frame 46 to rotate at a high speed.

In this embodiment, the packing layer placement frame 46 is cyclically kept stationary, the elastic sheet 464 is triggered, the packing layer placement frame 46 is rotated at a low speed, the packing layer placement frame 46 is rotated at a high speed, so that the reflux liquid is accumulated on the packing layer 47 in the step A2, the other components covered on the outer surface of chlorosulfonic acid on the surface of the packing layer 47 are dropped by the vibration of the elastic sheet 464 in the step A3, the gas phase and the liquid phase are further contacted, the packing layer placement frame 46 is driven to rotate at a low speed in the step A4, the gas phase and the liquid phase are driven to be fully and rapidly contacted, and finally the packing layer placement frame 46 is driven to rotate at a high speed in the step A5, so that the chlorosulfonic acid is centrifugally thrown out and flows downwards. The step performed by this cycle can sufficiently purify the bischlorosulfonyliminoacid.

In this embodiment, the first time, the second time, the third time, and the fourth time held in each of steps A3 to A5 may be obtained empirically or may be set fixedly, for example, for 10 minutes.

Example III

407kg of raw materials chlorosulfonyl isocyanate and 115L of chlorosulfonic acid are mixed in a tank, preheated to 60 ℃, air is replaced by nitrogen through a nitrogen replacement device before feeding, raw material mixed liquor is fed into a steam jacketed tubular reactor at a pressure of 1.0Mpa by a high-pressure plunger pump, the temperature of the tubular reactor is controlled at 100 ℃, after the reaction is finished, the raw material mixed liquor is pumped into an intermediate tank through the tubular reactor and then subjected to rectification, the temperature of the top of the tower is controlled at 110 ℃, a part of light components are returned to a recovery tank through a secondary condenser, a part of useless light components are subjected to three-waste treatment, and the dichlorosulfonylimide acid reaction liquor meeting the requirement of the tower kettle enters a reboiler and then reaches a product tank, thereby obtaining 272.2kg of high-purity dichlorosulfonylimide acid.

Example IV

407kg of raw materials chlorosulfonyl isocyanate and 115L of chlorosulfonic acid are mixed in a tank, preheated to 70 ℃, air is replaced by nitrogen through a nitrogen replacement device before feeding, raw material mixed liquor enters a steam jacket tubular reactor at a pressure of 1.0Mpa by a high-pressure plunger pump, the temperature of the tubular reactor is controlled to be 105 ℃, after the reaction is finished, the raw material mixed liquor is pumped to an intermediate tank through the tubular reactor and then subjected to rectification, the temperature of the top of the tower is controlled to be 105 ℃, a part of light components are returned to a recovery tank through a secondary condenser, a part of useless light components are subjected to three-waste treatment, and the reaction liquor of the dichlorosulfinic acid of which the tower kettle meets the requirements enters a reboiler and then reaches a product tank, thereby obtaining 260.8kg of high-purity dichlorosulfinic acid.

Example five

301kg of raw material chlorosulfonyl isocyanate and 86.25L of chlorosulfonic acid are mixed in a tank, preheated to 65 ℃, air is replaced by nitrogen by a nitrogen replacement device before feeding, raw material mixed solution enters a steam jacket tubular reactor at a pressure of 1.2Mpa by a high-pressure plunger pump, the temperature of the tubular reactor is controlled at 105 ℃, after the reaction is finished, the raw material mixed solution is pumped to an intermediate tank by the tubular reactor, rectification treatment is carried out, the temperature of the top of the tower is controlled at 100 ℃, a part of light components return to a recovery tank by a secondary condenser, a part of useless light components are subjected to three-waste treatment, and a dichlorosulfonylimide acid reaction solution meeting the requirement at the tower bottom enters a reboiler and then reaches a product tank to obtain 191.5kg of high-purity dichlorosulfonylimide acid.

Experimental data

The raw materials of chlorosulfonyl isocyanate and chlorosulfonic acid provided in the third, fourth and fifth embodiments are proportioned, and the reaction conditions are matched with the device for continuously preparing high-purity dichlorosulfonylimide acid provided in the first or second embodiment and the rectification tower matched control method in the device for continuously preparing high-purity dichlorosulfonylimide acid, rectification is carried out for 5 hours, finally the dichlorosulfonylimide acid is obtained at the bottom end of the tower body, the purity of the dichlorosulfonylimide acid prepared in the third, fourth and fifth embodiments is detected to be 99.5%, 98.7%, 97.6% in sequence, and the molar yield of the dichlorosulfonylimide acid prepared in the third, fourth and fifth embodiments is 73.5%, 70.1% and 68.8%. The ratio of chlorosulfonyl isocyanate and chlorosulfonic acid as raw materials provided in example one was explained as the optimum reaction conditions.

Through the proportion of raw materials chlorosulfonyl isocyanate and chlorosulfonic acid provided in the third embodiment, and the reaction conditions, the device for continuously preparing high-purity dichlorosulfonylimide acid according to the second embodiment is matched, wherein the rotating slurry continuously drives the filler layer placing frame to rotate for rectification for 5 hours (i.e. the control method provided by the above is not adopted), finally, the dichlorosulfonylimide acid is obtained at the bottom end of the tower body, the purity of the detected dichlorosulfonylimide acid is 97.4%, and the molar yield is 70.5%. The control method of the rectifying column according to the present application is described, and the purity and molar yield of the obtained dichlorosulfonyliminoacid can be improved.

It should be noted that in the claims, any reference signs placed between parentheses shall not be construed as limiting the claim. The word "comprising" does not exclude the presence of elements or steps not listed in a claim. The word "a" or "an" preceding an element does not exclude the presence of a plurality of such elements. The invention may be implemented by means of hardware comprising several distinct elements, and by means of a suitably programmed computer. In the unit claims enumerating several means, several of these means may be embodied by one and the same item of hardware. The use of the words first, second, third, etc. do not denote any order. These words may be interpreted as names.

While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.

In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.

In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms should not be understood as necessarily being directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.

Claims

1. A method for continuously preparing high-purity dichlorosulfonyliminoacid, which is characterized in that: the method comprises the following steps:

2. A method for continuously producing high-purity bischlorosulfonylimide acid according to claim 1, characterized in that: in step S2, heating the chlorosulfonyl isocyanate and chlorosulfonic acid mixture includes: the chlorosulfonyl isocyanate and chlorosulfonic acid mixture is fed into a tubular reactor at a flow rate of 2-5 kg/min, and the tubular reactor is used for heating the chlorosulfonyl isocyanate and chlorosulfonic acid mixture to 90-150 ℃.

3. A method for continuously producing high-purity bischlorosulfonylimide acid according to claim 1, characterized in that: in the step S3, the rectification and purification of the dichloro sulfinamic acid reaction solution comprises the following steps: purifying the dichloro sulfinamide acid reaction solution in a rectifying tower, wherein the negative pressure operation is carried out in the rectifying tower, and the temperature of the top of the rectifying tower is set to be 110-120 ℃.

4. A device for continuously preparing high-purity dichloro sulfonyl imide acid is characterized in that: comprising the following steps:

5. The apparatus for continuously producing high-purity bischlorosulfonylimide acid according to claim 4, wherein: the tubular reactor comprises:

6. The apparatus for continuously producing high-purity bischlorosulfonylimide acid according to claim 5, wherein: the back mixing structure comprises a locating plate arranged in the linear cavity tube, a hanging seat fixed in the locating plate, a spring locked on the hanging seat, a pushing ball arranged on the spring and a clamping cylinder for supporting the pushing ball.

7. The apparatus for continuously producing high-purity bischlorosulfonylimide acid according to claim 4, wherein: the rectifying column includes:

the tower body, the tower body top is provided with the steam outlet, the tower body bottom is provided with the liquid outlet, the tower body is close to the position of top and is provided with first inlet, the tower body is close to the position of bottom and is provided with the second inlet, the position in the middle of the tower body is provided with the third inlet, the tower body bottom is provided with the liquid outlet; the tower body is provided with a rotating device, the rotating device comprises a rotating motor arranged at the top end of the tower body, a rotating shaft arranged in the tower body, and a plurality of rotating paddles arranged in parallel on the rotating shaft, the rotating shaft is driven by the rotating motor, and the rotating shaft can be driven up and down so as to drive the rotating paddles to move up and down; a packing layer placing frame capable of moving up and down is hung above each rotating paddle in the tower body, a packing layer is placed in the packing layer placing frame, a plurality of backflow holes for backflow are formed in the bottom of the packing layer placing frame, through holes for enabling the rotating shafts to pass through are formed in the middle of the packing layer placing frame, the rotating paddles can support the packing layer placing frame after moving upwards so as to drive the packing layer placing frame to rotate together, and the rotating paddles can be separated from the bottom surface of the packing layer placing frame after moving downwards so that the packing layer placing frame is hung in the tower body and does not rotate;

8. The apparatus for continuously preparing high-purity bischlorosulfonylimide acid according to claim 7, wherein:

the bottom surface of the packing layer placing frame is provided with a plurality of radial elastic sheets which are connected in a single end mode and are opened downwards, the elastic sheets enable the bottom surface of the packing layer placing frame to present a plurality of openings, the size of each opening is configured to prevent the packing layer from falling down, the bottom surface of the packing layer placing frame is fixedly provided with a connecting block on the outer ring of each elastic sheet, the connecting block protrudes out of the bottom surface of the packing layer placing frame, and the protruding height of the connecting block is smaller than the height of the tail end of each opening;

9. The apparatus for continuously preparing high-purity bischlorosulfonylimide acid according to claim 7, wherein: the output shaft of the rotating motor and the rotating shaft are arranged in a sleeved mode in a sliding mode through a connecting seat, a screw rod assembly is arranged between the output shaft of the rotating motor and the rotating shaft and comprises a screw rod motor, a screw rod and a screw rod nut, the screw rod nut is fixedly connected with the connecting seat, the screw rod motor is fixedly arranged on the rotating shaft, the screw rod motor drives the screw rod nut to move up and down through the screw rod, so that the connecting seat is driven to move up and down, and the traction piece is hinged between the connecting seat and the baffle.

10. The apparatus for continuously preparing high-purity bischlorosulfonylimide acid according to claim 8, wherein: the control method of the rectifying tower comprises the following steps: