A Precisely Temperature-Controlled Distillation Column for Pharmaceutical Intermediates

Abstract

This utility model discloses a precision temperature-controlled pharmaceutical intermediate distillation column, addressing the problems of uneven heating, low temperature control accuracy, and insufficient cooling efficiency in traditional equipment by providing a novel structure. It includes a distillation column body (with an annular heating chamber containing a spiral flow channel and multiple drain holes), a double-spiral cooling pipe, internal and external thermometers, a spiral heat dissipation plate, and a propeller stirring unit. Through uniform distribution of heating oil, enhanced heat transfer via double-spiral cooling, temperature control based on internal and external temperature difference feedback, and increased contact area via the spiral heat dissipation plate, precise temperature control and efficient heat transfer are achieved, effectively improving product purity and yield, and facilitating maintenance.

Description

Technical Field

[0001] This utility model relates to the field of chemical separation equipment technology, and in particular to a pharmaceutical intermediate distillation tower with precise temperature control. Background Technology

[0002] Pharmaceutical intermediates are key intermediate products in drug synthesis, and their purity and quality directly affect the safety and efficacy of the final drug. Distillation, as one of the core processes for purifying pharmaceutical intermediates, requires extremely high precision in temperature control—temperature fluctuations can lead to material decomposition, byproduct formation, or loss of target components, thereby reducing product yield and purity. Currently, the distillation process of pharmaceutical intermediates mainly relies on traditional distillation equipment, but existing technologies have the following significant drawbacks: 1. Insufficient heating uniformity: Traditional distillation equipment often uses a single heating source (such as an electric heating mantle or bottom heating plate), and heat transfer relies on natural convection or simple flow guidance, which easily leads to uneven heating of the distillation tank. Excessively high local temperatures may cause material decomposition, while excessively low local temperatures result in low distillation efficiency and impurity residue. 2. Low cooling efficiency: The cooling systems of existing equipment are mostly single-pipe straight-out or simple spiral tube structures, with limited contact area between the coolant and the distillation tank, resulting in low heat exchange efficiency. This makes it difficult to quickly reduce the material temperature, prolonging the distillation cycle, increasing energy consumption, and increasing the residence time of materials in the high-temperature zone (which may lead to the loss of heat-sensitive components). 3. Delayed Temperature Monitoring: Traditional equipment typically only has a single temperature measuring point in the inner distillation tank or the outer heating tank, which cannot reflect the actual temperature distribution of the material inside the inner tank in real time (such as the temperature difference between the material layer and the tank wall). This results in a lack of precise basis for temperature control strategies (such as adjusting the heating oil flow rate), making it difficult to achieve dynamic and precise temperature control. 4. Low Heat Transfer and Mixing Efficiency: During distillation, the material is prone to sedimentation due to viscosity changes or local flow dead zones. The stirring system of traditional equipment is mostly a single-layer blade structure, which has limited mixing effect and affects the uniform transfer of heat and distillation efficiency. At the same time, material adhesion to the inner tank wall may increase the heat transfer resistance, further reducing the heat conduction efficiency.

[0003] In summary, there is an urgent need for a pharmaceutical intermediate distillation equipment with optimized structure, precise temperature control, efficient heat transfer, and easy maintenance to meet the pharmaceutical industry's production requirements for high purity and high stability of intermediates. Utility Model Content

[0004] The technical problem to be solved by this invention is to overcome the defects of the prior art and provide a pharmaceutical intermediate distillation tower with precise temperature control.

[0005] To solve the above-mentioned technical problems, this utility model provides the following technical solution:

[0006] This utility model discloses a precision temperature-controlled pharmaceutical intermediate distillation column, comprising: a distillation column body, with an inner distillation tank and a heating outer cylinder coaxially arranged inside, forming an annular heating chamber; at least one heating oil conduit is provided at the bottom of the heating chamber, and a heating oil solenoid valve is connected to the outside of the conduit; a heating oil outlet is provided at the top of the heating chamber, and a heating oil inlet is provided at the bottom, both connected to a heating oil supply system; a column cover is fixed at the top of the distillation column body, the column cover is connected to the top of the inner distillation tank, and a feed inlet is provided on the column cover; a slag discharge port is provided at the bottom of the distillation column body, connected to the bottom of the inner distillation tank; a cooling unit, including a cooling pipe extending through the center of the column cover into the inner distillation tank, the inlet of the cooling pipe being connected to the cooling liquid supply system via a cooling liquid solenoid valve, and the outlet being connected to the cooling liquid recovery system via a cooling liquid discharge valve; a temperature monitoring unit, including a first thermometer extending into the inner distillation tank and a second thermometer extending into the heating outer cylinder; a stirring unit, located inside the inner distillation tank, for driving material mixing; and a steam outlet is provided at the top of the column cover for outputting distillation steam.

[0007] As a preferred technical solution of this utility model, the inner wall of the heating outer cylinder is provided with a spiral guide channel. The guide channel extends along the axial direction of the heating outer cylinder and communicates with the drain hole of the heating oil conduit, so as to guide the heating oil to flow along the spiral trajectory to uniformly heat the distillation inner barrel.

[0008] As a preferred technical solution of this utility model, there are multiple heating oil conduits arranged evenly along the bottom of the distillation inner barrel. Each heating oil conduit has multiple drain holes on its side wall. The drain holes are evenly spaced along the axial direction of the conduit to uniformly inject heating oil into the heating chamber.

[0009] As a preferred embodiment of this utility model, the cooling pipe has a double spiral structure, including an inner spiral pipe and an outer spiral pipe. The inlet of the inner spiral pipe is connected to the coolant supply system, and the outlet is connected to the inlet of the outer spiral pipe. The outlet of the outer spiral pipe is connected to the coolant recovery system, forming a coolant return channel.

[0010] As a preferred embodiment of this utility model, a spiral heat dissipation plate is fixed on the inner wall of the distillation inner barrel. The heat dissipation plate extends along the axial direction of the distillation inner barrel and is welded and fixed to the inner wall of the distillation inner barrel to increase the contact area between the material and the inner barrel wall to enhance heat conduction.

[0011] As a preferred embodiment of this utility model, the stirring unit includes: a stirring shaft, which is vertically arranged inside the distillation inner tank and rotatably connected to the tower cover via a sealed bearing at its upper end; stirring blades, which are fixed to the lower end of the stirring shaft and have a propeller-like structure; a transmission assembly, which includes a driven wheel, a driving wheel, and a synchronous belt, wherein the driven wheel is fixed to the upper end of the stirring shaft, the driving wheel is fixed to the output shaft of the drive motor, and the synchronous belt connects the driven wheel and the driving wheel; and a drive assembly, which includes a drive motor fixed to the tower cover and a fixed bracket, wherein the fixed bracket is hinged to the tower cover and is used to support the drive motor; the drive motor drives the stirring shaft to rotate via the transmission assembly.

[0012] As a preferred technical solution of this utility model, the bottom of the heating outer cylinder is provided with an impurity discharge port, and the impurity discharge port is provided with a switchable slag discharge valve for cleaning the impurities deposited in the heating chamber.

[0013] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0014] 1. By setting up an annular heating chamber and designing a spiral guide channel on the inner wall of the heating outer cylinder (connected to the drain hole of the heating oil conduit), the heating oil flows evenly along the spiral trajectory. Combined with multiple heating oil conduits evenly arranged along the bottom of the inner cylinder (with multiple sets of drain holes on the side wall), the heating oil is evenly distributed in the circumference and axial direction of the inner cylinder, avoiding local overheating or overcooling, and ensuring that the overall temperature deviation of the inner cylinder is ≤±1℃ (verified by experiments), effectively preventing material decomposition or impurity generation.

[0015] 2. The cooling pipe adopts a double helix structure (the inner helix and the outer helix are connected in series), which extends the contact path between the coolant and the distillation tank and increases the heat exchange area. At the same time, the double helix structure forms a "supply-return" closed loop, which makes the coolant form a continuously flowing cold fluid layer around the inner tank, significantly improving the heat exchange efficiency. It can shorten the material cooling time after distillation by 30%-50% and reduce the loss of heat-sensitive components.

[0016] 3. By setting a first thermometer inserted into the distillation tank (monitoring the actual temperature of the material) and a second thermometer inserted into the heating outer cylinder (monitoring the temperature of the heating oil), and combining the temperature difference feedback between the two, the heating efficiency can be calculated in real time and the opening of the heating oil solenoid valve can be dynamically adjusted to achieve coordinated temperature control of "material temperature - heating oil temperature". This solves the problem that traditional single measuring point cannot reflect the true temperature distribution of the material, and the temperature control accuracy is improved to within ±0.5℃.

[0017] 4. The spiral heat dissipation plate on the inner wall of the distillation tank increases the contact area between the material and the tank wall, enhancing the heat transfer efficiency; the stirring unit adopts a propeller blade combined with synchronous belt drive design, which can generate axial and radial composite stirring flow, effectively breaking the dead zone of material deposition, avoiding material adhesion to the tank wall, and promoting uniform heat transfer, reducing energy consumption by about 20%. Attached Figure Description

[0018] The accompanying drawings are provided to further illustrate the present invention and form part of the specification. They are used together with the embodiments of the present invention to explain the present invention, but do not constitute a limitation thereof. In the drawings:

[0019] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0020] Figure 2 This is the front view of this utility model;

[0021] Figure 3 This is a cross-sectional structural diagram of the present invention;

[0022] Figure 4 This is a schematic diagram of the cooling unit in this utility model;

[0023] Figure 5 This is a schematic diagram of the heating oil conduit in this utility model;

[0024] In the diagram: 1. Distillation column body; 2. Cooling unit; 3. Stirring unit; 4. Column cover; 5. Steam outlet; 11. Distillation inner barrel; 12. Heating outer cylinder; 13. Heating chamber; 14. Heating oil conduit; 15. Heating oil solenoid valve; 16. Heating oil outlet; 17. Heating oil inlet; 18. Feed inlet; 19. Slag discharge port; 21. Cooling pipe; 22. Coolant solenoid valve; 23. Coolant discharge valve; 24. First thermometer; 25. Second thermometer; 31. Stirring shaft; 32. Stirring blades; 33. Driven wheel; 34. Synchronous belt; 35. Driving wheel; 36. Drive motor; 37. Fixed bracket; 111. Heat sink; 121. Flow guide channel; 122. Impurity discharge port; 123. Slag discharge valve; 141. Liquid discharge hole; 211. Inner spiral tube; 212. Outer spiral tube; 311. Sealed bearing. Detailed Implementation

[0025] The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0026] In the attached diagram, all identical reference numerals refer to the same components.

[0027] Example 1: Basic Precision Temperature Controlled Distillation Column for Pharmaceutical Intermediates

[0028] like Figure 1-5 As shown in the figure, this embodiment provides a precision temperature-controlled pharmaceutical intermediate distillation column with a basic structure, the core components of which and their connection relationships are as follows:

[0029] The distillation column 1 is a vertically arranged cylindrical body, with an inner distillation tank 11 and a heating outer tank 12 coaxially fixed inside, forming an annular heating chamber 13 between them. The inner distillation tank 11 is a cylindrical structure that runs vertically through the inside and has a smooth inner wall, used to hold the pharmaceutical intermediate materials to be distilled; the heating outer tank 12 is sleeved on the outside of the inner distillation tank 11 and is indirectly heated through an external heating oil circulation system.

[0030] At least one heating oil conduit 14 is provided at the bottom of the heating chamber 13, and a heating oil solenoid valve 15 (used to control the flow rate of heating oil) is fixedly connected to the outside of the conduit. A heating oil outlet 16 is provided at the top of the heating chamber 13, and a heating oil inlet 17 is provided at the bottom. The two are respectively connected to an external heating oil supply system (providing high-temperature heat transfer oil) through pipes to form a circulation path for heating oil: the high-temperature heat transfer oil enters the heating chamber 13 through the heating oil inlet 17, and is evenly injected into the heating chamber 13 through the drain hole of the heating oil conduit 14. The flow of heating oil can be optimized into a spiral trajectory (refer to embodiment 2), and finally flows back to the supply system from the heating oil outlet 16 to achieve uniform heating of the distillation inner tank 11.

[0031] The top of the distillation column 1 is fixedly connected to the column cover 4 via a flange. The column cover 4 communicates with the top opening of the inner distillation vessel 11 to ensure that the steam flows upward during the distillation process. The column cover 4 has a feed inlet 18 (for adding material to the inner distillation vessel 11) and a steam outlet 5 (for discharging the distilled steam). The bottom of the distillation column 1 has a slag discharge port 19, which communicates with the bottom of the inner distillation vessel 11 (after distillation, the material residue can be discharged through the slag discharge port 19).

[0032] Please see Figure 4 The cooling unit 2 includes a cooling pipe 21, a coolant solenoid valve 22, and a coolant discharge valve 23. The cooling pipe 21 can be a spiral or double spiral structure, preferably a double spiral design as in embodiment 3. It passes through the center of the tower cover 4 and extends into the interior of the distillation inner tank 11. Its inlet is connected to an external coolant supply system (such as low-temperature water or refrigerant) through the coolant solenoid valve 22, and its outlet is connected to a coolant recovery system through the coolant discharge valve 23. This is used to quickly remove the heat from the distillation inner tank 11 and achieve material cooling.

[0033] Please see Figure 3The temperature monitoring unit includes a first thermometer 24 and a second thermometer 25: the first thermometer 24 extends into the interior of the distillation inner barrel 11 (near the material layer) to monitor the material temperature in real time; the second thermometer 25 extends into the interior of the heating outer barrel 12 (near the heating oil) to monitor the heating oil temperature. Together, they provide data support for the temperature control system.

[0034] The stirring unit 3 is located inside the distillation inner tank 11 and includes a stirring shaft 31, a sealed bearing 311, a propeller-type stirring blade 32, a driven wheel 33, a driving wheel 35, a synchronous belt 34, and a drive motor 36. The stirring shaft 31 is vertically installed inside the distillation inner tank 11, and its upper end is rotatably connected to the tower cover 4 via the sealed bearing 311 (to ensure sealing). The stirring blade 32 is fixed to the lower end of the stirring shaft 31 and rotates to mix the materials. In the transmission assembly, the driven wheel 33 is fixed to the upper end of the stirring shaft 31, the driving wheel 35 is fixed to the output shaft of the drive motor 36, and the synchronous belt 34 connects the driven wheel 33 and the driving wheel 35 to achieve power transmission. The drive motor 36 is mounted on the top of the tower cover 4 via a fixed bracket 37, which is hinged to the tower cover 4 for easy angle adjustment to achieve stable support. Finally, it drives the stirring shaft 31 to rotate, preventing material sedimentation and enhancing heat transfer.

[0035] The bottom of the heating outer cylinder 12 is provided with an impurity discharge port 122. An on / off slag discharge valve 123 (such as a plug valve or gate valve) is provided at the impurity discharge port 122 to periodically clean the oxidized coking impurities deposited in the heating chamber 13 and prevent the conduit from becoming blocked or the heating from failing.

[0036] Example 2: Enhanced Heating Uniformity and Precision Temperature Control Distillation Column for Pharmaceutical Intermediates

[0037] Based on Example 1, this embodiment focuses on optimizing heating uniformity. The core improvement is in the structure of the spiral guide channel 121 of the heating outer cylinder 12 and the drain hole 141 of the heating oil conduit 14:

[0038] The inner wall of the heating outer cylinder 12 is machined with a spiral-shaped flow channel 121 (extending axially), which communicates with the drain hole 141 of the heating oil conduit 14. Specifically, there are multiple heating oil conduits 14 (e.g., 4) evenly arranged along the bottom of the distillation inner barrel 11, and each conduit has multiple drain holes 141 (evenly spaced along the axial direction) on its side wall. When the heating oil enters the heating chamber 13 through the heating oil inlet 17, it flows into the flow channel 121 through the drain hole 141 of the heating oil conduit 14, flowing along a spiral trajectory to form a double uniform distribution in both the circumferential and axial directions, avoiding local high or low temperature areas and ensuring that the circumferential temperature deviation of the distillation inner barrel 11 is ≤ ±1℃.

[0039] Example 3: High-efficiency cooling type precision temperature-controlled pharmaceutical intermediate distillation column

[0040] This embodiment, based on embodiment 1, focuses on optimizing cooling efficiency. Its core improvement is the double-helix structure of cooling pipe 21:

[0041] The cooling tube 21 adopts a double-helix design, including an inner helix 211 and an outer helix 212. The inlet of the inner helix 211 is connected to the coolant solenoid valve 22 (to receive low-temperature coolant), and the outlet is connected to the inlet of the outer helix 212; the outlet of the outer helix 212 is connected to the coolant discharge valve 23 (to the coolant recovery system). Both the inner and outer helixes are located inside the distillation inner tank 11, forming a "supply-return" closed loop: the low-temperature coolant first flows along the inner helix 211, initially absorbing heat from the inner tank, and then flows into the outer helix 212 for further heat exchange. This extends the contact path between the coolant and the inner tank, increases the heat exchange area, and shortens the material cooling time by 30%-50%, making it suitable for the rapid cooling requirements of heat-sensitive pharmaceutical intermediates.

[0042] The above embodiments, through different structural optimizations, all achieve precise temperature control, efficient heat transfer, and stable production in the distillation process of pharmaceutical intermediates. The appropriate embodiment structure can be selected according to the specific material characteristics (such as boiling point, viscosity, and heat sensitivity).

[0043] This invention relates to a precision temperature-controlled pharmaceutical intermediate distillation column. Through structural innovation, it achieves precise temperature control and efficient production of pharmaceutical intermediates, possessing excellent practicality and promotional value. Combined with intelligent control and material optimization, it can further improve the equipment's automation level, corrosion resistance, and energy utilization, meeting the pharmaceutical industry's demand for high-purity, high-stability intermediates.

[0044] Finally, it should be noted that the above description is merely a preferred embodiment of this utility model and is not intended to limit the utility model. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. A precisely temperature-controlled distillation column for pharmaceutical intermediates, characterized in that, include: The distillation column (1) has an inner distillation tank (11) and an outer heating cylinder (12) coaxially arranged inside, forming an annular heating chamber (13) between them; the bottom of the heating chamber (13) is provided with at least one heating oil conduit (14), and the outside of the conduit is connected to a heating oil solenoid valve (15); the top of the heating chamber (13) is provided with a heating oil outlet (16), and the bottom is provided with a heating oil inlet (17), which are respectively connected to the heating oil supply system; the top of the distillation column (1) is fixed with a column cover (4), which is connected to the top of the inner distillation tank (11), and the column cover (4) is provided with a feed inlet (18); the bottom of the distillation column (1) is provided with a slag discharge port (19), which is connected to the inner distillation tank. (11) Bottom connection; Cooling unit (2): includes a cooling pipe (21) that extends through the center of the tower cover (4) into the distillation inner barrel (11). The inlet of the cooling pipe (21) is connected to the cooling liquid supply system through the cooling liquid solenoid valve (22), and the outlet is connected to the cooling liquid recovery system through the cooling liquid discharge valve (23); Temperature monitoring unit: includes a first thermometer (24) that extends into the distillation inner barrel (11) and a second thermometer (25) that extends into the heating outer cylinder (12); Stirring unit (3): is set inside the distillation inner barrel (11) and is used to drive material mixing; The top of the tower cover (4) is provided with a steam outlet (5) for outputting distillation steam.

2. The pharmaceutical intermediate distillation column with precise temperature control according to claim 1, characterized in that, The inner wall of the heating outer cylinder (12) is provided with a spiral guide channel (121). The guide channel (121) extends along the axial direction of the heating outer cylinder (12) and communicates with the drain hole (141) of the heating oil conduit (14). It is used to guide the heating oil to flow along the spiral trajectory to uniformly heat the distillation inner barrel (11).

3. The pharmaceutical intermediate distillation column with precise temperature control according to claim 1, characterized in that, The heating oil conduits (14) are multiple and evenly arranged along the bottom of the distillation inner barrel (11). Each heating oil conduit (14) has multiple drain holes (141) on its side wall. The drain holes (141) are evenly spaced along the axial direction of the conduit and are used to evenly inject heating oil into the heating chamber (13).

4. The pharmaceutical intermediate distillation column with precise temperature control according to claim 1, characterized in that, The cooling pipe (21) has a double spiral structure, including an inner spiral pipe (211) and an outer spiral pipe (212). The inlet of the inner spiral pipe (211) is connected to the coolant supply system, and the outlet is connected to the inlet of the outer spiral pipe (212). The outlet of the outer spiral pipe (212) is connected to the coolant recovery system, forming a coolant return channel.

5. The pharmaceutical intermediate distillation column with precise temperature control according to claim 1, characterized in that, A spiral heat dissipation plate (111) is fixed on the inner wall of the distillation inner barrel (11). The heat dissipation plate (111) extends along the axial direction of the distillation inner barrel (11) and is welded and fixed to the inner wall of the distillation inner barrel (11) to increase the contact area between the material and the inner barrel wall to enhance heat conduction.

6. The pharmaceutical intermediate distillation column with precise temperature control according to claim 1, characterized in that, The stirring unit (3) includes: a stirring shaft (31), which is vertically installed inside the distillation tank (11) and its upper end is rotatably connected to the tower cover (4) through a sealed bearing (311); stirring blades (32), which are fixed to the lower end of the stirring shaft (31) and are propeller-type structures; a transmission assembly, which includes a driven wheel (33), a driving wheel (35) and a synchronous belt (34), wherein the driven wheel (33) is fixed to the upper end of the stirring shaft (31), the driving wheel (35) is fixed to the output shaft of the drive motor (36), and the synchronous belt (34) connects the driven wheel (33) and the driving wheel (35); a drive assembly, which includes a drive motor (36) fixed to the tower cover (4) and a fixed bracket (37), wherein the fixed bracket (37) is hinged to the tower cover (4) and is used to support the drive motor (36); the drive motor (36) drives the stirring shaft (31) to rotate through the transmission assembly.

7. The pharmaceutical intermediate distillation column with precise temperature control according to claim 1, characterized in that, The bottom of the heating outer cylinder (12) is provided with an impurity discharge port (122), and the impurity discharge port (122) is provided with a switchable slag discharge valve (123) for cleaning the impurities deposited in the heating chamber (13).

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