Rectification device for producing chlorosulfonyl isocyanate

Abstract

The utility model provides a rectification device for producing chlorosulfonyl isocyanate. The rectification device comprises a primary rectification tower and a secondary rectification tower, the primary rectifying tower comprises a tower body I, a filler layer I and an adjusting device capable of driving the filler layer I to rotate; the top of the tower body I is provided with a steam outlet I, the upper end of the side wall is provided with a tower top reflux inlet I, the bottom is provided with a kettle liquid outlet I, the lower end of the side wall is provided with a tower kettle reflux inlet I, one side of the middle section of the side wall is provided with a feed inlet I, and the other side of the middle section of the side wall is provided with a discharge outlet I; the secondary rectifying tower comprises a tower body II and a filler layer II; a steam outlet II is formed in the top of the tower body II; a tower top reflux inlet II is formed in the upper end of the side wall of the tower body II; a kettle liquid outlet II is formed in the bottom of the tower body II; according to the rectification device for producing the chlorosulfonyl isocyanate, disclosed by the utility model, a gas phase and a liquid phase can be fully contacted, the rectification and purification effects are good, and the yield of the chlorosulfonyl isocyanate is high.

Description

TECHNICAL FIELD

[0001] The utility model belongs to chlorosulfonyl isocyanate production equipment field, especially is involved in a kind of rectifying column for chlorosulfonyl isocyanate production. BACKGROUND

[0002] Chlorosulfonyl isocyanate is a very active intermediate. The substance reacts with hydroxyl, amino, carboxyl to generate N-chlorosulfonyl carbamic acid ester, urea, amide; it can add with water, active hydrogen, alcohol, phenol, amine, amide, carboxylic acid, olefin, aldehyde, ketone, ester, to obtain various new compounds, can be used as dehydrating agent, oxidizing agent. Chlorosulfonyl isocyanate is mainly used for producing cefuroxime, cefoxitin, carumonam and other drugs.

[0003] In the existing process, the synthesis of chlorosulfonyl isocyanate mainly adopts chlorocyan and sulfur trioxide reaction, and then the crude chlorosulfonyl isocyanate obtained by reaction is purified by rectification to obtain product chlorosulfonyl isocyanate. The reaction in the reaction system mainly includes the reaction of sulfur trioxide and chloro cyan to obtain chlorosulfonyl isocyanate, when sulfur trioxide is excessive, chloro pyrosulfonyl isocyanate is obtained, and chloro pyrosulfonyl isocyanate can be decomposed into chlorosulfonyl isocyanate and sulfur trioxide under heating condition, and chlorosulfonyl isocyanate and chloro pyrosulfonyl isocyanate will react to generate other byproducts. As can be known, on the one hand, there is a reaction of generating chlorosulfonyl isocyanate and sulfur trioxide in the reaction system, and on the other hand, there is a reaction of consuming chlorosulfonyl isocyanate, which affects the production purity of chlorosulfonyl isocyanate, and the existing rectification device has limited purification effect. In addition, the existing rectification tower structure has defects, the countercurrent liquid phase and gas phase have poor contact effect in the filler layer, the liquid phase layer is easily coated and stagnated in the filler layer, which affects the full contact with the gas phase, and finally affects the rectification and purification effect. UTILITY MODEL CONTENT

[0004] Therefore, to solve the above technical problems, the utility model provides a rectifying column for chlorosulfonyl isocyanate production, which has sufficient gas-liquid contact, good rectification and purification effect and high chlorosulfonyl isocyanate yield.

[0005] To achieve the above purpose, the technical scheme of the utility model is as follows:

[0006] A rectifying column for chlorosulfonyl isocyanate production, comprising:

[0007] A primary rectification tower, the primary rectification tower comprises a tower body one, a filler layer one arranged in the tower body one and an adjusting device capable of driving the filler layer one to rotate; the top of the tower body one is provided with a steam outlet one, the upper end of the side wall is provided with a tower top reflux port one, the bottom is provided with a kettle liquid outlet one, the lower end of the side wall is provided with a tower kettle reflux port one, one side of the middle segment of the side wall is provided with a feeding port one, and the other side of the middle segment of the side wall is provided with a discharging port one;

[0008] The secondary rectifying tower comprises a tower body two and a packing layer two arranged in the tower body two, the top of the tower body two is provided with a vapor outlet two, the upper end of the side wall is provided with a tower top reflux port two, the bottom is provided with a kettle liquid outlet two, the lower end of the side wall is provided with a tower kettle reflux port two, one side of the middle section of the side wall is provided with a feed inlet two connected with the discharge outlet one, and the other side of the middle section of the side wall is provided with a discharge outlet two.

[0009] In the primary rectifying tower, the reaction liquid is fed into the tower body one through the feed inlet one, the light component sulfur trioxide and cyanogen chloride are taken out from the vapor outlet one at the top of the tower body one, the high-boiling heavy phase component is taken out from the kettle liquid outlet one, and the mixture of chloro pyrosulfuryl isocyanate and chlorosulfonyl isocyanate is taken out from the discharge outlet one and fed into the secondary rectifying tower, so that the reaction in the tower body one is carried out in the direction of generating chloro pyrosulfuryl isocyanate and chlorosulfonyl isocyanate; in the secondary rectifying tower, chloro pyrosulfuryl isocyanate and chlorosulfonyl isocyanate are fed into the tower body two through the feed inlet two, the light component sulfur trioxide is taken out from the vapor outlet two at the top of the tower body two, a small amount of high-boiling heavy phase component is taken out from the kettle liquid outlet two, and the purified chlorosulfonyl isocyanate is taken out from the discharge outlet two, so that the chloro pyrosulfuryl isocyanate is decomposed into sulfur trioxide and chlorosulfonyl isocyanate in the direction of heat decomposition, and therefore, the high-purity chlorosulfonyl isocyanate product can be taken out from the discharge outlet two; in addition, the adjusting device arranged in the tower body one can rotate the packing layer one, so that the phenomenon of liquid phase stagnation covering the packing layer is reduced, the contact between the liquid phase and the gas phase is increased, and the mass transfer efficiency is improved.

[0010] Further, the inner side walls of the tower body one and the tower body two are each provided with a circumferential slot; the packing layer one and the packing layer two each comprise an outer frame which can be inserted into the slot and a packing which is filled in the outer frame.

[0011] The packing layer and the slot are detachably connected, so that the later maintenance is facilitated.

[0012] Further, the slot has a plurality of vertical equidistant distribution; the packing layer one has a plurality of one-to-one corresponding installation in the tower body one; the packing layer two has a plurality of one-to-one corresponding installation in the tower body two.

[0013] The packing layer adopts a modular structure and is arranged at intervals, so that the situation of extrusion and damage of the packing layer is reduced.

[0014] Further, the adjusting device comprises a driving motor mounted on the outside of a top of the tower body, a rotating shaft vertically arranged in an inner cavity of the tower body and connected with the output end of the driving motor, a vertical insertion channel is arranged in the central position of the first packing layer for the rotating shaft to pass through, and a clamping groove is arranged in the lower section of the insertion channel; and a clamping block is fixedly arranged on the rotating shaft and can be clamped in the clamping groove.

[0015] The driving motor can drive the rotating shaft to rotate, the clamping block is arranged on the rotating shaft and embedded in the clamping groove of the first packing layer, so that the first packing layer can be driven to rotate when the rotating shaft rotates, the liquid phase covering the first packing layer is thrown away, and the contact efficiency of the gas-liquid two-phase is improved.

[0016] Further, a plurality of universal rollers are arranged at the positions corresponding to the insertion grooves of the bottom of the first packing layer and are equidistantly arranged in the circumferential direction.

[0017] The universal rollers are arranged to make the first packing layer more easily rotate under the driving of the rotating shaft.

[0018] Further, the adjusting device comprises a driving motor mounted on the outside of a top of the tower body, a rotating shaft vertically arranged in an inner cavity of the tower body and connected with the output end of the driving motor, a vertical insertion channel is arranged in the central position of the first packing layer for the rotating shaft to pass through, and a clamping groove is arranged in the lower section of the insertion channel; and a clamping block is fixedly arranged on the rotating shaft and can be clamped in the clamping groove.

[0019] Compared with the prior art, the rectifying device for chlorosulfonyl isocyanate production has the following advantages:

[0020] (1) The rectifying device for chlorosulfonyl isocyanate production has a reasonable structure design, two-stage rectifying towers are arranged, the system can be controlled to react in the direction of generating chlorosulfonyl isocyanate, the rectifying and purifying effect is good, and the yield of chlorosulfonyl isocyanate is high.

[0021] (2) The rectifying device for chlorosulfonyl isocyanate production is provided with an adjusting device for adjusting the first packing layer in the tower body, the phenomenon that the liquid phase is stagnantly covered on the first packing layer can be reduced, the gas phase and the liquid phase are fully contacted, and the mass transfer efficiency is improved. BRIEF DESCRIPTION OF DRAWINGS

[0022] The accompanying drawings, which form a part of this patent, are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the principles of the application. In the drawings:

[0023] Figure 1 The structure schematic view of rectifying device for chlorosulfonyl isocyanate production of the present application;

[0024] Figure 2 The structure schematic view of the clamping groove of the present application;

[0025] Figure 3 The structure schematic view of the clamping block of the present application;

[0026] Figure 4 The structure schematic view of Figure 1 The enlarged view of A of the structure schematic view of

[0027] Marked for the drawings:

[0028] 1 - primary rectifying tower, 2 - condenser one, 3 - reboiler one, 4 - secondary rectifying tower, 5 - condenser two, 6 - reboiler two, 7 - tower body one, 8 - filler layer one, 9 - steam outlet one, 10 - tower top reflux port one, 11 - kettle liquid outlet one, 12 - tower kettle reflux port one, 13 - feed inlet one, 14 - discharge port one, 15 - slot, 16 - outer frame, 17 - filler, 18 - universal roller, 19 - driving motor, 20 - rotating shaft, 21 - clamping groove, 22 - clamping block, 23 - tower body two, 24 - filler layer two, 25 - steam outlet two, 26 - tower top reflux port two, 27 - kettle liquid outlet two, 28 - tower kettle reflux port two, 29 - feed inlet two, 30 - discharge port two. DETAILED DESCRIPTION

[0029] It should be noted that the embodiments in the present application and the features in the embodiments can be combined with each other without conflict.

[0030] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", etc. are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, features defined as "first", "second", etc. may explicitly or implicitly include one or more of the features. In the description of the present invention, unless otherwise specified, "multiple" means two or more.

[0031] In the description of this utility model, it should be noted that, unless otherwise expressly specified or limited, the terms "installed," "connected," and "connected" should be understood in a broad sense. For example, they can refer to fixed connections, detachable connections, or integral connections; mechanical connections, electrical connections; direct connections, indirect connections through an intermediate medium, and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in this utility model based on specific circumstances.

[0032] The present invention will be described in detail below with reference to the accompanying drawings and in combination with embodiments.

[0033] like Figures 1 to 4 As shown, a distillation device for producing chlorosulfonyl isocyanate includes a primary distillation tower 1, a condenser 2, a reboiler 3, a secondary distillation tower 4, a condenser 5 and a reboiler 6;

[0034] The primary rectifying tower 1 comprises a tower body 7, a filler layer 8 arranged in the tower body 7, and an adjusting device capable of driving the filler layer 8 to rotate; the top of the tower body 7 is provided with a steam outlet 9, the upper end of the side wall is provided with a tower top reflux port 10, the bottom is provided with a kettle liquid outlet 11, the lower end of the side wall is provided with a tower kettle reflux port 12, one side of the middle section of the side wall is provided with a feed inlet 13, and the other side of the middle section of the side wall is provided with a discharge outlet 14; the inner side wall of the tower body 7 is provided with a circumferential slot 15; the filler layer 8 comprises an outer frame 16 capable of being inserted into the slot 15 and fillers 17 filled in the outer frame 16; a plurality of universal rollers 18 are installed at the bottom of the filler layer 8 and correspond to the positions of the slots 15 in the circumferential direction; the slots 15 are arranged in the vertical direction at equal intervals; the filler layer 8 comprises a plurality of filler layers, which are installed in the tower body 7 in one-to-one correspondence; the adjusting device comprises a driving motor 19 installed on the outside of the top of the tower body 7 and a rotating shaft 20 vertically arranged in the inner cavity of the tower body 7 and connected with the output end of the driving motor 19; the central position of the filler layer 8 is provided with a vertical through slot for the rotating shaft 20 to pass through, and the lower section of the through slot is provided with a clamping groove 21; the rotating shaft 20 is fixedly sleeved with a clamping block 22 capable of being clamped in the clamping groove 21;

[0035] The condenser 2 is connected with the steam outlet 9 and the tower top reflux port 10, and is used for condensing the light component steam at the top of the tower body 7 and refluxing part of the condensed liquid;

[0036] The reboiler 3 is connected with the kettle liquid outlet 11 and the tower kettle reflux port 12, and is used for heating and vaporizing the heavy component liquid at the tower kettle of the tower body 7, and refluxing part of the steam;

[0037] The secondary rectifying tower 4 comprises a tower body 23 and a filler layer 24 arranged in the tower body 23; the top of the tower body 23 is provided with a steam outlet 25, the upper end of the side wall is provided with a tower top reflux port 26, the bottom is provided with a kettle liquid outlet 27, the lower end of the side wall is provided with a tower kettle reflux port 28, one side of the middle section of the side wall is provided with a feed inlet 29 connected with the discharge outlet 14, and the other side of the middle section of the side wall is provided with a discharge outlet 30; the inner side wall of the tower body 23 is provided with a circumferential slot 15; the filler layer 24 comprises an outer frame 16 capable of being inserted into the slot 15 and fillers 17 filled in the outer frame 16; the slots 15 are arranged in the vertical direction at equal intervals; the filler layer 24 comprises a plurality of filler layers, which are installed in the tower body 23 in one-to-one correspondence;

[0038] The condenser 5 is connected with the steam outlet 25 and the tower top reflux port 26, and is used for condensing the light component steam at the top of the tower body 23 and refluxing part of the condensed liquid;

[0039] The reboiler 6 is connected with the kettle liquid outlet 27 and the tower kettle reflux port 28, and is used for heating and vaporizing the heavy component liquid at the tower kettle of the tower body 23, and refluxing part of the steam.

[0040] The working process of the rectification device for chlorosulfonyl isocyanate production is as follows:

[0041] In the primary rectification tower 1, the reaction liquid is sent into the tower body 7 through the feed port 13; the light component sulfur trioxide and cyanogen chloride which are not completely reacted are taken out from the top vapor outlet 9 of the tower body 7, condensed by the condenser 2, and then refluxed through the tower top reflux port 10; the high-boiling heavy phase component generated by the side reaction is taken out from the kettle liquid outlet 11, vaporized by the reboiler 3, and then refluxed through the tower kettle reflux port 12; the gas-liquid phase countercurrent contact is adopted, the mixture of chloro pyrosulfonyl isocyanate and chlorosulfonyl isocyanate is taken out from the discharge port 14, and then sent into the secondary rectification tower 4;

[0042] In the secondary rectification tower 4, the chloro pyrosulfonyl isocyanate and the chlorosulfonyl isocyanate are sent into the tower body 23 through the feed port 29; the light component sulfur trioxide generated by the decomposition of the chloro pyrosulfonyl isocyanate is taken out from the top vapor outlet 25 of the tower body 23, condensed by the condenser 5, and then refluxed through the tower top reflux port 26; the small amount of high-boiling heavy phase component is taken out from the kettle liquid outlet 27, vaporized by the reboiler 6, and then refluxed through the tower kettle reflux port 28; and the purified chlorosulfonyl isocyanate is taken out from the discharge port 30;

[0043] Since the adjusting device which can rotate the packing layer 8 is arranged in the tower body 7, when the liquid phase is stagnantly coated on the packing layer 8, the driving motor 19 can drive the rotating shaft 20 to rotate, the clamping block 22 on the rotating shaft 20 is clamped in the clamping groove 21, and then the packing layer 8 can be driven to rotate, so that the liquid phase stagnantly coated on the packing layer 8 is thrown away.

[0044] The above only describes the preferred embodiments of the present application, and is not used to limit the present application, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A distillation device for producing chlorosulfonyl isocyanate, characterized in that: The application relates to a distillation tower. The first-stage distillation tower comprises a tower body one, a filler layer one arranged in the tower body one and an adjusting device capable of driving the filler layer one to rotate; the top of the tower body one is provided with a steam outlet one, the upper end of the side wall is provided with a tower top reflux port one, the bottom is provided with a kettle liquid outlet one, the lower end of the side wall is provided with a tower kettle reflux port one, one side of the middle section of the side wall is provided with a feeding port one, and the other side of the middle section of the side wall is provided with a discharging port one; the second-stage distillation tower comprises a tower body two and a filler layer two arranged in the tower body two; the top of the tower body two is provided with a steam outlet two, the upper end of the side wall is provided with a tower top reflux port two, the bottom is provided with a kettle liquid outlet two, the lower end of the side wall is provided with a tower kettle reflux port two, one side of the middle section of the side wall is provided with a feeding port two connected with the discharging port one, and the other side of the middle section of the side wall is provided with a discharging port two. The inner side walls of the tower body one and the tower body two are provided with circumferential insertion grooves; the filler layer one and the filler layer two each comprise an outer frame which can be inserted into the insertion grooves and a filler filled in the outer frame.

2. The rectifying apparatus for producing chlorosulfonyl isocyanate according to claim 1, characterized by: The insertion grooves are vertically and equidistantly distributed; the filler layer one comprises a plurality of filler layers which are installed in the tower body one one by one; the filler layer two comprises a plurality of filler layers which are installed in the tower body two one by one.

3. The rectifying apparatus for producing chlorosulfonyl isocyanate according to claim 2, characterized by: The adjusting device comprises a driving motor installed on the outside of the top of the tower body one and a rotating shaft vertically arranged in the inner cavity of the tower body one and connected with the output end of the driving motor; the central position of the filler layer one is provided with a vertical through insertion channel through which the rotating shaft passes; the lower section of the through insertion channel is provided with a clamping groove; a clamping block which can be clamped in the clamping groove is fixedly arranged on the rotating shaft.

4. The rectifying device for chlorosulfonyl isocyanate production according to claim 2, characterized by: A plurality of universal rollers are circumferentially and equidistantly arranged at the positions corresponding to the insertion grooves of the bottom of the filler layer one.

5. The rectifying apparatus for producing chlorosulfonyl isocyanate according to claim 4, characterized by: The application further comprises a condenser one, a reboiler one, a condenser two and a reboiler two; the condenser one is connected with the steam outlet one and the tower top reflux port one, is used for condensing light component steam on the top of the tower body one, and refluxes part of the condensed liquid; the reboiler one is connected with the kettle liquid outlet one and the tower kettle reflux port one, is used for heating and vaporizing heavy component liquid in the tower kettle of the tower body one, and refluxes part of the steam; the condenser two is connected with the steam outlet two and the tower top reflux port two, is used for condensing light component steam on the top of the tower body two, and refluxes part of the condensed liquid; and the reboiler two is connected with the kettle liquid outlet two and the tower kettle reflux port two, is used for heating and vaporizing heavy component liquid in the tower kettle of the tower body two, and refluxes part of the steam.

6. The rectifying apparatus for producing chlorosulfonyl isocyanate according to any one of claims 1 to 5, characterized by: ​

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