Vacuum distillation device for preparing medical intermediate

Abstract

The utility model relates to the technical field of production of medical intermediates, in particular to a vacuum distillation device for preparing medical intermediates. Comprising a tank body, a heater is fixed in the tank body, the upper end of the tank body is communicated with a cooling tank through a pipeline, the upper end of the cooling tank is communicated with a vacuum pump, a rotating rod is rotationally connected in the tank body, a plurality of inverted-U-shaped branch pipes are fixed to the outer edge of the rotating rod, an inner hole is concentrically formed in the rotating rod, the inner hole is communicated with the branch pipes, and the lower end of the inner wall of a straight part below the branch pipes is flush with the bottom of the inner hole. The side, facing the side wall of the tank body and the side, facing the center of the tank body, of the vertical part of each branch pipe are each provided with a plurality of spray holes, and the upper side and the lower side of the straight part of each branch pipe are each provided with a plurality of spray holes. After the materials in the tank body are discharged, the materials in the inner holes of the branch pipe and the rotating rod can flow out through the spraying holes in the lower side of the straight part below the branch pipe, and the materials can be prevented from being retained in the branch pipe and the inner holes.

Description

Technical Field

[0001] The utility model relates to the technical field of pharmaceutical intermediate production, in particular to a vacuum distillation device for pharmaceutical intermediate production. Background Art

[0002] Pharmaceutical intermediate p-toluenesulfonyl isocyanate is an important organic chemical intermediate, mainly used as a pharmaceutical intermediate for the synthesis of hypoglycemic drugs such as glimepiride, gliclazide, glipizide, etc., for the treatment of type 2 diabetes. In the pesticide field, it can be used to synthesize sulfonylurea herbicides, etc.

[0003] The patent document with application number 202210131439.2 and titled "A method for preparing p-toluenesulfonyl isocyanate" discloses a preparation method that uses dimethyl carbonate as a reaction raw material to replace the highly toxic phosgene for a synthesis reaction, which is highly safe and can meet the synthesis requirements without the need for high-pressure reaction equipment. The method comprises the following steps: (1) Chlorination reaction: Add dimethyl carbonate to a reactor and introduce chlorine gas for a chlorination reaction.

[0004] (2) Esterification reaction: p-toluenesulfonamide is dissolved in chlorobenzene to form a p-toluenesulfonamide chlorobenzene solution, the p-toluenesulfonamide chlorobenzene solution is added to the reaction kettle, and refluxed at 90-110° C. for 3-5 hours.

[0005] (3) Purification: After the esterification reaction is completed, the reaction product is subjected to reduced pressure to recover chlorobenzene, and the reaction product after recovering the chlorobenzene is subjected to high vacuum distillation to obtain p-toluenesulfonyl isocyanate.

[0006] In step (3), a vacuum distillation device is required. Some existing vacuum distillation devices do not have a cleaning function and it is inconvenient to clean the inside of the distillation device.

[0007] The patent document with application number 202322072828.5 and titled "A Low-temperature Vacuum Distillation Device" discloses a vacuum distillation device that is convenient for cleaning the inside of the vacuum distillation device. In actual application, the liquid is first preheated by the preheating device and then enters the distillation tank, which can shorten the heating time and make the liquid heated evenly. After the liquid enters the distillation tank, the vacuum pump is used to evacuate the distillation tank to keep the inside of it in a vacuum state, the heating plate heats the liquid in the tank, the stirring motor drives the driving gear to rotate, the driving gear drives the driven gear ring to rotate through the tooth chain, and then drives the stirring shaft and the stirring frame to rotate, so as to clean the inside of the distillation tank. The liquid is stirred so that the liquid is heated more evenly, further shortening the distillation time. The gas separated by distillation enters the condenser through the outlet pipe on the upper part of the distillation tank to condense into liquid. The concentrated liquid separated by distillation is discharged through the drain pipe at the bottom of the distillation tank. After the distillation is completed, the one-way valve is opened, and the external cleaning liquid enters the stirring frame through the pipeline connected to the stirring shaft, and the inner wall of the distillation tank is cleaned through the one-way valve. While the cleaning liquid is entering, the stirring motor drives the stirring shaft and the stirring frame to rotate, and the inner wall of the distillation tank can be rotated and sprayed for cleaning, which is convenient for cleaning and effectively saves cleaning liquid. The distillation time of the utility model is short, time cost and cleaning liquid are saved, and cleaning is convenient. In this technical solution, by setting a one-way valve, it is possible to prevent the material from entering the stirring frame when the material is stirred. The one-way valve needs to be opened during cleaning. Multiple one-way valves are set on the stirring frame. When cleaning the inside of the distillation device, the one-way valve will lose part of the pressure of the high-pressure flushing liquid, thereby reducing the pressure inside the device under the action of the cleaning liquid. At the same time, multiple one-way valves are provided, and the cleaning fluid cannot be effectively discharged after the one-way valve is blocked, thereby increasing the maintenance cost. Utility Model Content

[0008] The technical problem to be solved by the utility model is to provide a spare vacuum distillation device for a pharmaceutical intermediate system which has low maintenance cost and can ensure the flushing pressure of the cleaning liquid on the inside of the device.

[0009] In order to achieve the above purpose, the technical solution provided by the utility model is:

[0010] A vacuum distillation device for pharmaceutical intermediates includes a tank body, a heater is fixed in the tank body, the upper end of the tank body is connected to a cooling tank through a pipeline, the upper end of the cooling tank is connected to a vacuum pump, a rotating rod is rotatably connected in the tank body, a plurality of inverted U-shaped branch pipes are fixed on the outer edge of the rotating rod, an inner hole is concentrically opened in the rotating rod, the inner hole is connected to the branch pipe, the lower end of the inner wall of the straight part below the branch pipe is flush with the bottom of the inner hole, a plurality of spray holes are opened on the side of the vertical part of the branch pipe facing the side wall of the tank body and the side facing the center of the tank body, and the straight part of the branch pipe There are multiple spray holes on the upper and lower sides. A motor is fixed on the upper end of the tank body. The output shaft of the motor is fixedly connected to the rotating rod. The rotating rod passes through the output shaft of the motor. A connecting sleeve is provided on the rotating sealing sleeve on the rotating rod above the motor. The connecting sleeve is fixed on the motor. The connecting sleeve is connected to the inner hole of the rotating rod. The connecting sleeve is fixedly connected to the inlet pipe, and the inlet pipe is connected to the cleaning equipment. The vertical part of the branch pipe is fixedly connected to the rotating rod through multiple connecting rods. The angle between the axis of the spray holes on the upper and lower sides of the connecting rod and adjacent to the connecting rod and the axis of the connecting rod is 10°~15°.

[0011] Specifically, the upper end of the tank body is fixedly connected with a feeding pipe, and the lower end of the tank body is fixedly connected with a discharging pipe, and valves are installed on the feeding pipe and the discharging pipe.

[0012] Specifically, the connecting sleeve is fixedly connected to the motor via a plurality of supporting rods.

[0013] Specifically, a vent valve is fixedly connected to the connecting sleeve.

[0014] Specifically, a valve is installed on the inlet pipe.

[0015] Specifically, a plurality of communication holes are provided on the rotating rod inside the communication sleeve, and the communication sleeve is connected with the inner hole of the rotating rod through the plurality of communication holes.

[0016] Specifically, a condenser is installed in the cooling tank.

[0017] Specifically, the angle between the axis of the spray holes on the upper and lower sides of the connecting rod and adjacent to the connecting rod and the axis of the connecting rod is 10°.

[0018] Compared with the prior art, the beneficial effects of the utility model are:

[0019] 1. When the branch pipe stirs the material in the tank, the material can enter the inner hole of the branch pipe and the rotating rod through the spray hole. By limiting the positional relationship between the straight part below the branch pipe and the bottom of the inner hole, the lower end of the inner wall of the straight part below the branch pipe is flush with the bottom of the inner hole. After the material in the tank is discharged, the material in the inner hole of the branch pipe and the rotating rod can flow out through the spray hole on the lower side of the straight part below the branch pipe, which can avoid material retention in the branch pipe and the inner hole.

[0020] 2. By setting the vent valve, the tank is in a vacuum state. When the vent valve is opened, the outside air enters the tank through the inner hole, branch pipe and spray hole, and the materials in the branch pipe and inner hole can be completely removed.

[0021] 3. The angle between the spray holes on the upper and lower sides of the connecting rod and adjacent to the connecting rod and the axis of the connecting rod is 10° to 15°. The cleaning fluid sprayed from the spray holes on the upper and lower sides of the connecting rod and adjacent to the connecting rod can focus on flushing the connecting rod. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a schematic diagram of the utility model.

[0023] Figure 2 for Figure 1 Magnified view of area C.

[0024] Figure 3 for Figure 1 Magnified view of area A.

[0025] Figure 4 This is a schematic diagram of the coordination between the rotating rod and the branch pipe.

[0026] Figure 5 It is a top view of the cooperation between the branch pipe and the rotating rod.

[0027] Figure 6 for Figure 5 B-section view in the figure.

[0028] Figure 7 for Figure 6 Schematic diagram of region D in center.

[0029] Figure 8 Schematic diagram of the spray holes on the upper and lower sides of the connecting rod and adjacent to the connecting rod.

[0030] The names of the parts in the attached drawings are:

[0031] 1 Tank

[0032] 2 Heater

[0033] 3 Cooling tank

[0034] 4 Vacuum pump

[0035] 5 Rotating rod

[0036] 501 inner hole

[0037] 6 branches

[0038] 601 nozzle

[0039] 7 Connecting rod

[0040] 8 Motor

[0041] 9 Support rod

[0042] 10 Inlet pipe

[0043] 11 Connecting hole

[0044] 12 Vent valve

[0045] 13 Connected sets. DETAILED DESCRIPTION

[0046] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments.

[0047] Example 1: Reference Figure 1-Figure 7 As shown, a vacuum distillation device for a pharmaceutical intermediate system includes a tank body 1, in which a heater 2 is fixed. A feeding pipe is fixedly connected to the upper end of the tank body 1, and a discharge pipe is fixedly connected to the lower end of the tank body 1. Valves are installed on the feeding pipe and the discharge pipe. The heater 2 can heat the material in the tank body 1. Material can be added to the tank body 1 through the feeding pipe. The material in the tank body 1 can be discharged through the discharge pipe.

[0048] The upper end of the tank body 1 is connected to the cooling tank 3 through a pipeline, and the upper end of the cooling tank 3 is connected to the vacuum pump 4. A condenser is installed in the cooling tank 3.

[0049] The vacuum pump 4 is started to keep the vacuum degree in the cooling tank 3 consistent with that in the tank body 1, and the heater 2 is used to heat the material in the tank body 1. The impurities in the material are converted into steam and then volatilized into the cooling tank 3 and condensed by the condenser in the cooling tank 3.

[0050] A rotating rod 5 is rotatably connected inside the tank body 1, and a plurality of inverted U-shaped branch pipes 6 are fixed to the outer edge of the rotating rod 5. An inner hole 501 is concentrically opened inside the rotating rod 5, and the inner hole 501 is connected to the branch pipe 6. The lower end of the inner wall of the straight part below the branch pipe 6 is flush with the bottom of the inner hole 501.

[0051] The vertical part of the branch pipe 6 is provided with a plurality of spray holes 601 on one side facing the side wall of the tank body 1 and on one side facing the center of the tank body 1. The straight part of the branch pipe 6 is provided with a plurality of spray holes 601 on both upper and lower sides. A motor 8 is fixed on the upper end of the tank body 1. The output shaft of the motor 8 is fixedly connected to the rotating rod 5. The rotating rod 5 passes through the output shaft of the motor 8. A connecting sleeve 13 is provided on the rotating rod 5 above the motor 8. The connecting sleeve 13 is fixedly connected to the motor 8 through a plurality of support rods 9. A plurality of connecting holes 11 are provided on the rotating rod 5 inside the connecting sleeve 13. The connecting sleeve 13 is connected to the inner hole 501 of the rotating rod 5 through the plurality of connecting holes 11. The connecting sleeve 13 is fixedly connected to the inlet pipe 10. The inlet pipe 10 is connected to the cleaning equipment. A valve is installed on the inlet pipe 10. The vertical part of the branch pipe 6 is fixedly connected to the rotating rod 5 through a plurality of connecting rods 7.

[0052] When the motor 8 drives the rotating rod 5, the branch pipe 6 and the connecting rod 7 to rotate, the branch pipe 6 and the connecting rod 7 can stir the material in the tank body 1. When stirring the material, the material can enter the branch pipe 6 and the inner hole 501 of the rotating rod 5 through the spray hole 601. After the material in the tank body 1 is discharged, the material in the branch pipe 6 and the inner hole 501 can be discharged through the spray hole 601 of the straight part below the branch pipe 6 under the action of gravity. Since the lower end of the inner wall of the straight part below the branch pipe 6 is flush with the bottom of the inner hole 501, it can prevent the material from remaining in the branch pipe 6 and the inner hole 501.

[0053] When it is necessary to clean the inside of the tank body 1, the cleaning device is started, and the cleaning device allows the cleaning liquid to be sprayed out through the inlet pipe 10, the connecting sleeve 13, the connecting hole 11, the inner hole 501, the branch pipe 6 and the spray hole 601. The cleaning liquid sprayed from the spray hole 601 can clean the inside of the tank body 1, and the cleaning liquid sprayed from the spray hole 601 can also clean the rotating rod 5.

[0054] When cleaning the inside of the tank body 1, the motor 8 is started, and the motor 8 drives the rotating rod 5, the branch pipe 6 and the connecting rod 7 to rotate. The rotating branch pipe 6 and the connecting rod 7 are in contact with the mist-like cleaning liquid in the tank body 1, which can further improve the cleaning efficiency of the branch pipe 6 and the connecting rod 7. During the rotation of the rotating rod 5, the connecting sleeve 13 is connected with the inner hole 501 through the connecting hole 11.

[0055] Embodiment 2, based on embodiment 1, refer to Figure 8 As shown, the angle between the axis of the spray holes 601 on the upper and lower sides of the connecting rod 7 and the axis of the connecting rod 7 is 10° to 15°. Preferably, the angle between the axis of the spray holes 601 on the upper and lower sides of the connecting rod 7 and the axis of the connecting rod 7 is 10°.

[0056] In this embodiment, in order to ensure the cleaning efficiency of the connecting rod 7, the axial angle of the spray hole 601 on the upper and lower sides of the connecting rod 7 and adjacent to the connecting rod 7 is limited, and the cleaning liquid sprayed from the spray hole 601 on the upper and lower sides of the connecting rod 7 and adjacent to the connecting rod 7 can focus on flushing the connecting rod 7.

[0057] Based on Example 1, refer to Figure 3 As shown, the communication sleeve 13 is fixedly connected with a vent valve 12 .

[0058] In this embodiment, in order to ensure that the materials in the branch pipe 6 and the inner hole 501 are completely discharged, a vent valve 12 is fixedly connected to the connecting sleeve 13. The vacuum state in the tank body 1 is maintained, and then the vent valve 12 is opened, and the air outside the tank body 1 enters the tank body 1 through the vent valve 12, the connecting sleeve 13, the connecting hole 11, the inner hole 501, the branch pipe 6 and the spray hole 601. In the process of air flowing in the inner hole 501 and the branch pipe 6, the materials in the branch pipe 6 and the inner hole 501 can be further blown away, which can ensure that the materials are completely discharged from the inner hole 501 and the branch pipe 6.

[0059] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A vacuum distillation device for pharmaceutical intermediates, comprising a tank body (1), a heater (2) fixed inside the tank body (1), an upper end of the tank body (1) connected to a cooling tank (3) through a pipeline, and an upper end of the cooling tank (3) connected to a vacuum pump (4), characterized in that: A rotating rod (5) is rotatably connected inside the tank body (1), a plurality of inverted U-shaped branch pipes (6) are fixed to the outer edge of the rotating rod (5), an inner hole (501) is coaxially opened inside the rotating rod (5), the inner hole (501) is communicated with the branch pipe (6), the lower end of the inner wall of the straight portion below the branch pipe (6) is flush with the bottom of the inner hole (501), a plurality of spray holes (601) are opened on the side of the vertical portion of the branch pipe (6) facing the side wall of the tank body (1) and the side facing the center of the tank body (1), and a plurality of spray holes (601) are opened on both upper and lower sides of the straight portion of the branch pipe (6), a motor (8) is fixed to the upper end of the tank body (1), and the output shaft of the motor (8) is connected to the rotating rod. (5) is fixedly connected, the rotating rod (5) passes through the output shaft of the motor (8), a connecting sleeve (13) is provided on the rotating rod (5) above the motor (8), the connecting sleeve (13) is fixed on the motor (8), the connecting sleeve (13) is connected with the inner hole (501) of the rotating rod (5), the connecting sleeve (13) is fixedly connected with the inlet pipe (10), the inlet pipe (10) is connected with the cleaning equipment, the vertical part of the branch pipe (6) is fixedly connected with the rotating rod (5) through a plurality of connecting rods (7), and the angle between the axis of the spray hole (601) on the upper and lower sides of the connecting rod (7) and adjacent to the connecting rod (7) and the axis of the connecting rod (7) is 10° to 15°.

2. The vacuum distillation device for pharmaceutical intermediate production according to claim 1, characterized in that: The upper end of the tank body (1) is fixedly connected to a feeding pipe, and the lower end of the tank body (1) is fixedly connected to a discharging pipe, and valves are installed on the feeding pipe and the discharging pipe.

3. The vacuum distillation device for pharmaceutical intermediate preparation according to claim 1, characterized in that: The connecting sleeve (13) is fixedly connected to the motor (8) via a plurality of supporting rods (9).

4. The vacuum distillation device for pharmaceutical intermediate production according to claim 1, characterized in that: The communication sleeve (13) is fixedly connected with a vent valve (12).

5. The vacuum distillation device for pharmaceutical intermediate production according to claim 1, characterized in that: A valve is installed on the inlet pipe (10).

6. The vacuum distillation device for pharmaceutical intermediate production according to claim 1, characterized in that: A plurality of communication holes (11) are provided on the rotating rod (5) inside the communication sleeve (13), and the communication sleeve (13) is connected to the inner hole (501) of the rotating rod (5) through the plurality of communication holes (11).

7. The vacuum distillation device for pharmaceutical intermediate production according to claim 1, characterized in that: A condenser is installed in the cooling tank (3).

8. The vacuum distillation device for pharmaceutical intermediate production according to claim 1, characterized in that: The angle between the axis of the spray holes (601) located on the upper and lower sides of the connecting rod (7) and adjacent to the connecting rod (7) and the axis of the connecting rod (7) is 10°.

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