A preparation device and method of medrogestrel

Abstract

The invention discloses a preparation device and method of medrogestrel. The device comprises a premixing tank, a mixing device, and a reaction device. After reaction materials are sequentially added to the reaction device in a plurality of set cycles, the temperature of the reaction chamber is maintained constant and aeration is continuously performed for 30-60 minutes, and then the reaction enters a recrystallization stage. Then, the aerator is stopped, and the upper and lower heating blocks are controlled to cool to 40-50°C at a rate of 2-5°C / min, and the temperature is maintained at 40-50°C until recrystallization is completed. After the crystallization is completed, the recrystallized primary product is taken out through a discharge port provided at the right bottom of the reaction device and placed in a washing device, washed with excess 2-propanol in the washing device, and the washing liquid is discharged after washing is completed. Then, the primary product is dried in the washing device to obtain medrogestrel.

Description

Technical Field

[0001] The present invention relates to the technical field of medrogestrel preparation, and in particular to a device and method for preparing medrogestrel. Background Art

[0002] Medrogestrel is a 6-methyl steroid commonly used to treat certain diseases caused by female menstruation. It is generally produced by recrystallizing a progesterone extract initially inoculated with mesosulfuronone seeds. Currently, the products on the market are basically produced by foreign manufacturers. Domestic manufacturers can basically only complete the manufacturing of intermediates or primary products for the preparation of medrogestrel. The preparation of medrogestrel by recrystallization is only in the laboratory preparation stage and cannot form industrial preparation. Summary of the Invention

[0003] In order to solve the problems of the prior art, the present invention provides a preparation device for medrogestrel, comprising:

[0004] Premix tank, used for premixing the progesterone extract and dipropylene glycol in a set ratio to form a primary premix;

[0005] The mixing device is used to add the primary premix in the premix tank in a quantitative manner according to a set period and fully mix it according to a set rule under the control of the control device to form a reaction material; the reaction material is added to the reaction device in batches according to the set period;

[0006] The reaction device is used to spray the uniformly mixed reaction materials in the form of fine particles into a reaction chamber provided in the reaction device through a dispersion pipe, and then the upper heating block and the lower heating block provided at the upper and lower ends of the reaction chamber are heated and kept boiling until the reaction materials are completely dissolved; during the dissolution of the reaction materials, preheated inert gas is introduced through at least one group of aerators provided at the bottom of the reaction chamber, so that the reaction materials are accelerated in the explosive gas of the inert gas to be fully dissolved, and the steam formed and the floating inert gas are input into the reflux cooling device through the guide pipe provided at one end of the reaction device, and the steam is condensed by the reflux cooling device and then input into the liquid collecting tank, and at the same time, a drainage groove is formed in the reflux cooling device to recover the inert gas to the gas collection tank;

[0007] After the reaction materials are sequentially added to the reaction device in multiple set cycles, the temperature of the reaction chamber is maintained unchanged and the explosion is continued for 30-60 minutes, and then the process enters the recrystallization stage. The aerator is then stopped, and the upper and lower heating blocks are controlled to cool to 40-50°C at a rate of 2-5°C / min, and maintained at 40-50°C until the recrystallization is completed. After the crystallization is completed, the recrystallized primary product is taken out through the discharge port provided at the right bottom of the reaction device and placed in a washing device, washed with excess 2-propanol in the washing device, and the washing liquid is discharged after washing is completed. The primary product is then dried in the washing device to obtain medrogestrel.

[0008] Furthermore, the premixing tank is connected to the first dosing tank and the second dosing tank respectively.

[0009] Furthermore, the mixing device

[0010] The mixing shell comprises a mixing space formed inside the mixing shell, and a pushing piston is provided at one left end of the mixing shell, the left side of the pushing piston is connected to a push rod, and the push rod is provided on the pushing cylinder, and a feed port, a discharge port and a reflux port are provided on the mixing shell, a feed valve is provided at the feed port, the premixing tank is connected to the feed valve through a premixing pipeline, and a pressure control valve is provided at the discharge port, and the pressure control valve is connected to the reaction device through a feed pipeline.

[0011] Furthermore, the reaction device includes a reactor shell, an isolation plate arranged on the left side inside the reactor shell, a reaction chamber is formed on the right side of the isolation plate and inside the reactor shell, an upper heating block and a lower heating block are respectively arranged at the upper and lower ends of the reaction chamber, and at least one set of aerators is arranged at the bottom of the reaction chamber, the aerators are connected to the preheating tank through the explosion pipeline and the explosion control valve, and the preheating tank is connected to the gas source tank; on the right side of the reaction chamber, a baffle is arranged against the inner wall of the reaction chamber, and a A guide port is provided at the guide port. A guide filter is provided at the right side of the guide filter. A guide pipe is integrated with the reactor shell. A guide channel is formed inside the guide pipe, and a guide plate is provided inside the guide channel. The guide plate is provided on the right side of the guide filter, and the guide plate divides the guide channel into an upper guide groove and a lower ventilation groove. An air increase pipe is provided at the bottom of the guide pipe and located at the lower ventilation groove, and the air increase pipe is connected to the gas source tank through an air increase pipeline; the end of the guide channel is connected to the reflux cooling device.

[0012] Furthermore, the reflux cooling device is a three-stage cooling device, including a first-stage condensation component in which a multi-stage composite membrane is arranged; a second-stage air drainage diversion component connected to the first-stage condensation component and a third-stage air drainage diversion component connected to the second-stage air drainage diversion component; the end of the three-stage air drainage diversion component is connected to the liquid collecting tank through a diversion pipeline, and the liquid collecting tank is connected to the reflux port through a reflux pipeline and a reflux valve.

[0013] Furthermore, the first-stage condensing assembly, the second-stage evacuation and diversion assembly, and the third-stage evacuation and diversion assembly are three independent units connected in sequence;

[0014] The first stage condensing assembly includes: a condensing outer shell and a condensing inner tube, a closed first cooling channel is formed between the condensing outer shell and the condensing inner tube, and a first inlet and a first outlet are opened on the condensing outer shell, the first inlet is connected to the cold water tank through a first flow control valve and a first water inlet pipeline, and the first outlet is connected to the recovery water tank through a second flow control valve and a first return pipeline;

[0015] The replacement speed of the cooling water in the first cooling channel is controlled by setting the opening of the first flow control valve and the second flow control valve, so as to control the cooling degree of the steam and the inert gas by the first condensing component;

[0016] The steam passing through the multi-stage composite membrane arranged in the first-stage condensation inner tube is condensed on the mesh during the condensation process. After condensing into water droplets, the water droplets are accelerated to penetrate the multi-stage composite membrane under the action of the inert gas and enter the second-stage gas drainage and diversion component. The inert gas freely passes through the multi-stage composite membrane and enters the interior of the second-stage gas drainage and diversion component.

[0017] The two-stage air evacuation and diversion assembly includes: a two-stage condensation outer shell and a two-stage condensation inner tube, the two-stage condensation inner tube is configured to have a first groove with a downward inclination at the bottom, the first groove is used to transport condensed water to the three-stage air evacuation and diversion assembly, and the upper part of the two-stage condensation inner tube is configured to have a first diversion groove with an upward inclination, and the inert gas is collected into the gas collection tank through the first diversion groove; a second cooling channel is formed between the two-stage condensation outer shell and the two-stage condensation inner tube, a second inlet and a second outlet are opened on the two-stage condensation outer shell, the second inlet is connected to the cold water tank through a third flow control valve and a second water inlet pipeline, and the second outlet is connected to the recovery water tank through a fourth flow control valve and a second return pipeline; and the replacement speed of the cooling water in the second cooling channel is controlled by setting the opening of the third flow control valve and the fourth flow control valve, so as to achieve the control of the cooling degree of the steam and the inert gas by the two-stage condensation assembly;

[0018] The three-stage air evacuation and diversion assembly includes: a three-stage condensation outer shell and a three-stage condensation inner tube, the three-stage condensation inner tube is configured to have a second groove with a downward inclination at the bottom, the second groove is used to transport condensed water to the end of the three-stage condensation inner tube, and the upper part of the three-stage condensation inner tube is configured to have a second diversion groove with an upward inclination, and the inert gas is collected into the gas collection tank through the second diversion groove; a third cooling channel is formed between the three-stage condensation outer shell and the three-stage condensation inner tube, a third inlet and a third outlet are opened on the three-stage condensation outer shell, the third inlet is connected to the cold water tank through the fifth flow control valve and the third water inlet pipeline, and the third outlet is connected to the recovery water tank through the sixth flow control valve and the third return pipeline; and the replacement speed of the cooling water in the third cooling channel is controlled by setting the opening of the fifth flow control valve and the sixth flow control valve, so as to achieve the control of the cooling degree of the three-stage condensation assembly on the steam and the inert gas;

[0019] The first groove and the second groove have the same inclination, and the first groove and the second groove are connected at the end.

[0020] Furthermore, the control device controls the feed valve to open according to a set period, feeds a set amount of primary premix into the mixing space from the premix tank, then controls the feed valve and the return valve to close respectively, and then sets the upper limit value for triggering the pressure control valve; the control device controls the pushing cylinder to push the push rod within the set period according to the set periodic control instruction set to drive the pushing piston to reciprocate in the mixing space, and within the set period, the pushing stroke of the pushing piston in the mixing space gradually increases, so that the primary premix in the mixing space is evenly mixed during the reciprocating motion of the pushing piston, and when the pushing stroke gradually increases, the pressure environment in the mixing space is also gradually increased, and the gradual increase in the pressure environment accelerates the mixing of the primary premix, and when at the end of the execution of the set period, the pushing stroke of the pushing piston gradually reaches When it reaches the maximum, the pressure in the mixing space reaches the upper limit value triggered by the pressure control valve. At this time, the pressure control valve is opened, and the evenly mixed primary premix forms a reaction material, which is transported to the reaction device under the action of the propulsion piston, and the evenly mixed reaction material is sprayed into the reaction chamber provided in the reaction device in the form of fine particles through the dispersion pipe provided in the reaction device; when the pressure in the mixing space drops below the upper limit value triggered by the pressure control valve, the pressure control valve is closed, and the pressure control valve sends a feedback instruction to the control device. When the control device receives the feedback instruction, the control device controls the feed valve to open again according to the set cycle, and feeds a set amount of primary premix into the mixing space from the premix tank, and then controls the feed valve and the reflux valve to be closed respectively, and controls the mixing device to complete the control of the control instruction set for the next cycle.

[0021] Furthermore, the first dosing tank and the second dosing tank are connected to the premixing tank respectively through a first metering valve and a second metering valve and correspondingly arranged delivery pipelines.

[0022] The present invention also provides a method for preparing medrogestrel, comprising the following steps:

[0023] Step 1) adding 50 kg of progesterone extract mixed with mesosulfuronone seed crystals and 230 L of diacetone from the first dosing tank and the second dosing tank to the premixing tank respectively through the first metering valve and the second metering valve; then slowly stirring for 5-8 hours through the premixing tank;

[0024] Step 2) The control device controls the feed valve to open according to the set period, and feeds a set amount of primary premix into the mixing space from the premix tank, then controls the feed valve and the return valve to close respectively, and then sets the upper limit value of the triggering of the pressure control valve; the control device controls the pushing cylinder to push the push rod within the set period according to the set periodic control instruction set to drive the pushing piston to reciprocate in the mixing space, and within the set period, the pushing stroke of the pushing piston in the mixing space gradually increases, so that the primary premix in the mixing space is evenly mixed during the reciprocating motion of the pushing piston, and when the pushing stroke gradually increases, the pressure environment in the mixing space is also gradually increased, and the gradual increase in the pressure environment accelerates the mixing of the primary premix. At the end of the execution of the set period, the pushing cylinder is pushed When the propulsion stroke of the material piston gradually reaches the maximum, the pressure in the mixing space reaches the upper limit value triggered by the pressure control valve. At this time, the pressure control valve is opened, and the evenly mixed primary premix forms a reaction material, which is transported to the reaction device under the action of the propulsion piston. The evenly mixed reaction material is sprayed into the reaction chamber provided in the reaction device in the form of fine particles through the dispersion pipe provided in the reaction device; when the pressure in the mixing space drops below the upper limit value triggered by the pressure control valve, the pressure control valve is closed, and the pressure control valve sends a feedback instruction to the control device. When the control device receives the feedback instruction, the control device controls the feed valve to open again according to the set cycle, and feeds a set amount of primary premix into the mixing space from the premix tank, and then controls the feed valve and the reflux valve to close respectively;

[0025] Step 3) Repeat step 2) to spray the uniformly mixed reaction materials obtained in multiple cycles into a reaction chamber provided in the reaction device in the form of fine particles until all the primary premix is ​​added to the mixing device and transferred from the mixing device to the reaction device;

[0026] Step 4) The reaction material sprayed in the form of fine particles is heated and kept boiling in the reaction chamber by upper and lower heating blocks arranged at the upper and lower ends of the reaction chamber until the reaction material is completely dissolved; during the dissolution of the reaction material, preheated inert gas is introduced through at least one set of aerators arranged at the bottom of the reaction chamber to accelerate the movement of the reaction material in the explosive gas of the inert gas to fully dissolve it, and the steam generated and the floating inert gas are input into the reflux cooling device through a guide pipe arranged at one end of the reaction device. The steam is condensed by the reflux cooling device and then input into the liquid collecting tank. At the same time, a drainage groove is formed in the reflux cooling device to recover the inert gas to the gas collection tank;

[0027] Step 5) After the reaction materials are sequentially added to the reaction device in multiple set cycles, the reaction chamber temperature is maintained unchanged and the gas is exploded for 30-60 minutes, entering the recrystallization stage, and then the aerator is stopped, and the upper and lower heating blocks are controlled to cool to 40-50°C at a rate of 2-5°C / min, and maintained at 40-50°C until the recrystallization is completed. After the crystallization is completed, the recrystallized primary product is taken out through the discharge port provided at the bottom right of the reaction device and placed in a washing device, and washed with excess 2-propanol in the washing device. After washing, the washing liquid is discharged, and then the primary product is dried in the washing device to obtain medrogestrel.

[0028] After step 3) is completed, the control device controls the reflux valve to open, and the recovered liquid collected in the liquid collecting tank enters the mixing device through the reflux valve, reflux pipeline, and reflux port. The pushing piston is controlled to reciprocate in the mixing space to mix the liquid evenly again and then input into the reaction device.

[0029] This application uses a surging method to achieve uniform mixing of materials. Compared to stirring, surging allows for a more uniform distribution of solids during solid-liquid suspension. Stirring, on the other hand, tends to cause solids to gather in a central vortex, which is detrimental to uniform distribution. Furthermore, as the piston pushes forward, the pressure within the mixing space gradually increases, which also accelerates mixing.

[0030] During the dissolution of the reaction materials, preheated inert gas is introduced through at least one set of aerators disposed at the bottom of the reaction chamber, causing the reaction materials to accelerate in the explosive atmosphere of the inert gas, thereby fully dissolving. Simultaneously, the generated vapor and the rising inert gas are fed into a reflux cooling device through a draft tube disposed at one end of the reaction apparatus. The vapor is condensed by the reflux cooling device and then fed into a liquid collecting tank. Simultaneously, a diversion groove is formed within the reflux cooling device to recover the inert gas to a gas collection tank. Nitrogen is preferably used as the inert gas, and its preheating temperature is 180-220°C. That is, when nitrogen is introduced, the temperature in the reaction chamber does not drop, and the reaction chamber can still maintain a boiling state. The inert gas can accelerate the churning of the reaction materials within the reactor, thereby fully dissolving the reaction materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0032] Figure 1 It is a structural schematic diagram of the device provided by the present invention;

[0033] Figure 2 It is a schematic structural diagram of the assembled reaction device and reflux cooling device provided by the present invention. DETAILED DESCRIPTION

[0034] To make the objectives, technical solutions and advantages of the present invention more clear, the embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.

[0035] Example 1, with reference to Figure 1 and Figure 2 The present invention provides a preparation device for medrogestrel, comprising:

[0036] The premixing tank 5 is used to premix the progesterone extract and dipropylene glycol in a set ratio to form a primary premix; the mixing device is used to quantitatively add the primary premix in the premixing tank 5 according to a set period under the control of the control device and fully mix it according to a set rule to form a reaction material; the reaction material is added to the reaction device 20 in sequence according to the set period; the reaction device 20 is used to spray the uniformly mixed reaction material in the form of fine particles into the reaction chamber provided in the reaction device 20 through a dispersion tube, and then heated and kept boiling by the upper heating block 204 and the lower heating block 207 provided at the upper and lower ends of the reaction chamber until the reaction material is completely dissolved; during the dissolution process of the reaction material, preheated inert gas is introduced through at least one group of aerators provided at the bottom of the reaction chamber to accelerate the movement of the reaction material in the explosion of the inert gas to fully dissolve, and the vapor formed and the floating inert gas are The liquid is fed into the reflux cooling device 6 through a guide pipe provided at one end of the reaction device 20, and the steam is condensed by the reflux cooling device 6 and fed into the liquid collecting tank. At the same time, a drainage groove is formed in the reflux cooling device 6 to recover the inert gas to the gas collection tank. After the reaction materials are sequentially added to the reaction device 20 in multiple set cycles, the temperature of the reaction chamber is kept unchanged and the explosion is continued for 30-60 minutes, and then enters the recrystallization stage. Then, the aerator is stopped, and the upper heating block 204 and the lower heating block 207 are controlled to cool to 40-50°C at a rate of 2-5°C / min, and maintained at 40-50°C until the recrystallization is completed. After the crystallization is completed, the recrystallized primary product is taken out through the discharge port provided at the bottom right side of the reaction device 20 and placed in a washing device, washed with excess 2-propanol in the washing device, and the washing liquid is discharged after washing. Then, the primary product is dried in the washing device to obtain medrogestrel.

[0037] In the above, the premixing tank 5 is connected to the first dosing tank 3 and the second dosing tank 4, respectively; and the first dosing tank 3 and the second dosing tank 4 are connected to the premixing tank 5 through the first metering valve 30 and the second metering valve 40 and the corresponding transmission pipelines. In the present application, the premixing tank 5 adopts a stirring tank with stirring. 50 kg of progesterone extract mixed with mesulfuronone seed crystals is added to the premixing tank 5 from the first dosing tank 3 through the first metering valve 30. At the same time, the second metering valve 40 is opened, 230 L of diacetone is added to the premixing tank 5, and then slowly stirred for 5-8 hours through the premixing tank 5.

[0038] In the above, the mixing device includes a mixing shell 13, a mixing space 14 is formed inside the mixing shell 13, and a pushing piston 15 is provided at the left end of the mixing shell 13, and the left side of the pushing piston 15 is connected to the push rod 12, and the push rod 12 is provided on the pushing cylinder 1, and a feed port 17, a discharge port and a reflux port 18 are provided on the mixing shell 13, and a feed valve 50 is provided at the feed port 17. The premixing tank 5 is connected to the feed valve 50 through a premixing pipeline, and a pressure control valve 16 is provided at the discharge port, and the pressure control valve 16 is connected to the reaction device 20 through the feed pipeline 2. During mixing, the control device controls the feed valve 50 to open according to a set period, and feeds a set amount of primary premix into the mixing space 14 from the premix tank, then controls the feed valve 50 and the return valve 71 to close respectively, and then sets the upper limit value for triggering the pressure control valve 16; the control device controls the pushing cylinder 1 to push the push rod 12 within a set period according to a set set of periodic control instructions to drive the pushing piston 15 to reciprocate in the mixing space 14, and within the set period, the pushing stroke of the pushing piston 15 in the mixing space 14 gradually increases, so that the primary premix in the mixing space 14 is evenly mixed during the reciprocating motion of the pushing piston 15, and when the pushing stroke gradually increases, the pressure environment in the mixing space 14 is also gradually increased. The gradual increase in the pressure environment accelerates the mixing of the primary premix, and at the end of the execution of the set period, the pushing stroke of the pushing piston 15 gradually increases. When it gradually reaches the maximum, the pressure in the mixing space 14 reaches the upper limit value triggered by the pressure control valve 16. At this time, the pressure control valve 16 is opened, and the evenly mixed primary premix forms a reaction material, which is transported to the reaction device 20 under the action of the propulsion piston, and the evenly mixed reaction material is sprayed into the reaction chamber provided in the reaction device 20 in the form of fine particles through the dispersion pipe provided in the reaction device 20; when the pressure in the mixing space 14 drops below the upper limit value triggered by the pressure control valve 16, the pressure control valve 16 is closed, and the pressure control valve 16 sends a feedback instruction to the control device. When the control device receives the feedback instruction, the control device controls the feed valve 50 to open again according to the set cycle, and feeds a set amount of primary premix into the mixing space 14 from the premix tank, and then controls the feed valve 50 and the reflux valve 71 to be closed respectively, and controls the mixing device to complete the control of the control instruction set for the next cycle.

[0039] In the above, the set cycle is a 30-minute cycle, including the control device controlling the feed valve 50 to open according to the 30-minute cycle, and feeding a set amount of primary premix into the mixing space 14 from the premix tank, for example, adding 10L of primary premix at a time, and then controlling the feed valve 50 and the reflux valve 71 to be closed respectively, and then setting the upper limit value for triggering the pressure control valve 16 (for example, set to 5-15Kpa); wherein, the upper limit value for triggering the pressure control valve 16 only needs to be set once before starting the machine, and the pressure control valve 16 can be implemented by the following methods, one is to set a group of pressure sensors on the inner wall of the mixing space 14, and collect the pressure in the mixing space 14 in real time through the pressure sensors, and transmit the collected pressure data to the control device, the control device receives the pressure data and compares it with the set upper limit value for triggering the pressure control valve 16 to determine whether it exceeds, if it exceeds, the pressure control valve 16 is controlled to open, if it exceeds, the pressure control valve 16 is controlled to remain closed. The pressure control valve 16 adopts an intelligent control type solenoid valve and is connected to the control device. Another solution is to adopt an adaptive pressure regulating valve to perform automatic control.

[0040] In the above, the periodic control instruction set refers to the same as the above-mentioned set cycle (cycled once every 30 minutes), that is, the control instruction set also cycles once every 30 minutes, and completes the execution of one cycle of instructions within 30 minutes, wherein the control instruction set is an instruction set for controlling the pushing cylinder 1, for example, one instruction is executed every 3 minutes, and within the first 3 minutes, the pushing cylinder 1 pushes the pushing piston 15 forward through the push rod 12 with a maximum stroke of 5 units (which can be actually converted into a specific distance), and drives the pushing piston 15 to reciprocate in the mixing space 14 within 3 minutes, and the pushing piston 15 reciprocates in the mixing space 14. During movement, the primary premix in the corresponding mixing space 14 is uniformly mixed in the form of back and forth surge (simulating the ebb and flow of the tide). When the pushing piston 15 moves forward, the pressure in the mixing space 14 gradually increases. The increase in pressure also accelerates the uniform mixing of the materials. In the second 3 minutes, the maximum stroke of the pushing piston 15 pushed forward by the pushing cylinder 1 through the push rod 12 is 10 units, and so on, until the 10th 3 minutes is executed, the maximum stroke of the pushing piston 15 pushed forward by the pushing cylinder 1 through the push rod 12 is 50 units. At this time, the pushing stroke is the maximum, and the upper limit value of the triggering pressure control valve 16 is reached.

[0041] The present application uses a surging method to achieve uniform mixing of materials. Compared to the stirring method, the surging method makes the solid distribution more uniform when the solid-liquid suspension is in place. However, during stirring, the solids tend to gather in the central vortex of the stirring, which is not conducive to uniform distribution of the solids. In addition, the pressure in the mixing space 14 gradually increases due to the piston's advancement, which also accelerates the mixing process.

[0042] In the above, the reaction device 20 includes a reactor shell, an isolation plate 205 arranged on the left side inside the reactor shell, a reaction chamber is formed on the right side of the isolation plate 205 and inside the reactor shell, an upper heating block 204 and a lower heating block 207 are respectively arranged at the upper and lower ends of the reaction chamber, and at least one group of aerators are arranged at the bottom of the reaction chamber, the aerators are connected to the preheating tank 23 through the explosion pipeline and the explosion control valve, and the preheating tank 23 is connected to the gas source tank 22; on the right side of the reaction chamber, a baffle is arranged against the inner wall of the reaction chamber, a guide port is arranged on the upper part of the baffle, and a guide port is arranged at the guide port. A guide filter 200 is provided, and on the right side of the guide filter 200 is a guide pipe integrated with the reactor shell. A guide channel is formed inside the guide pipe, and a guide plate 202 is provided inside the guide channel. The guide plate 202 is provided on the right side of the guide filter 200, and the guide plate 202 divides the guide channel into an upper guide groove 203 and a lower ventilation groove. An air increase pipe 216 is provided at the bottom of the guide pipe and located at the lower ventilation groove, and the air increase pipe 216 is connected to the preheating tank through an air increase pipeline and an air increase control valve 215; the end of the guide channel is connected to the reflux cooling device 6.

[0043] In the above, a dispersion tube 206 is provided on the right side of the isolation plate 205, through which the evenly mixed reaction materials are sprayed into the reaction chamber provided in the reaction device 20 in the form of refined particles; wherein a plurality of dispersion holes are provided on the dispersion tube, and the instantaneous power during dispersion is provided by the pushing piston 15 after reaching the maximum stroke.

[0044] In the above, a group of aerators includes a first aerator 209 and a second aerator 212. The bottoms of the first aerator 209 and the second aerator 212 are respectively provided with a first explosion control valve 208 and a second explosion control valve 210. The first explosion control valve 208 and the second explosion control valve 210 are connected to the control device and are controlled to open and close by the control device.

[0045] In the above, the interior of the preheating tank 23 has a preheating inner tube, which forms a preheating space. A heating space 230 is formed between the preheating inner tube and the preheating tank shell, and a heating component is arranged in the heating space. This is the same as the structure of the existing heating tank on the market, and the existing heating tank can be directly used.

[0046] In the above, the uniformly mixed reaction materials obtained in multiple cycles are sprayed into the reaction chamber provided in the reaction device 20 in the form of fine particles until the primary premix is ​​completely added to the mixing device and transferred from the mixing device to the reaction device 20; the reaction materials sprayed in the form of fine particles are heated in the reaction chamber by the upper heating block 204 and the lower heating block 207 provided at the upper and lower ends of the reaction chamber and kept boiling (temperature of 180-220° C.) until the reaction materials are completely dissolved; during the dissolution process of the reaction materials, preheated inert gas is introduced through at least one set of aerators provided at the bottom of the reaction chamber to accelerate the movement of the reaction materials in the explosive gas of the inert gas so as to fully dissolve, and the steam formed and the floating inert gas are input into the reflux cooling device 6 through the guide pipe provided at one end of the reaction device 20, and the steam is condensed by the reflux cooling device 6 and input into the liquid collecting tank, and at the same time, a drainage groove is formed in the reflux cooling device 6 to recover the inert gas to the gas collection tank 29. The inert gas is preferably nitrogen, and its preheating temperature is 180-220°C. That is, when nitrogen is filled in, the temperature in the reaction chamber will not drop and it can still maintain a boiling state. The inert gas can accelerate the churning of the reaction materials inside the reactor to fully dissolve them.

[0047] In the above, the inert gas in the reaction chamber and the steam of the stroke enter the guide pipe through the guide port through the filter screen. In order to accelerate the movement of the inert gas and steam in the guide pipe, and to provide a certain pressure to the reflux cooling device 6 as needed (so that after the steam condenses into liquid, it can accelerate the liquid to permeate the multi-stage composite membrane and enter the second-stage gas diversion assembly under the action of the inert gas), nitrogen is injected into the guide pipe at the bottom of the guide pipe through the air increase pipe 216. Among them, the baffle is set in an L shape to guide the inert gas and steam to move up and down in the guide pipe, and a gas channel 201 is set between the baffle and the inner wall of the guide pipe. The nitrogen introduced from the bottom can flow into the guide pipe from the gas channel 201 to add to the diversion of the inert gas and steam.

[0048] In the above description, the reflux cooling device 6 is a three-stage cooling device, comprising a first-stage condensing assembly, within which a multi-stage composite membrane 602 is disposed; a second-stage degassing and diversion assembly connected to the first-stage condensing assembly; and a third-stage degassing and diversion assembly connected to the second-stage degassing and diversion assembly; the ends of the three-stage degassing and diversion assemblies are connected to the liquid collecting tank 7 via a diversion pipeline and a diversion valve 72, and the liquid collecting tank 7 is connected to the reflux port 18 via a reflux pipeline, a reflux control valve 70, and a reflux valve 71. The multi-stage composite membrane 602 is composed of multiple composite membranes arranged in intervals, and is constructed using a metal grid and a multi-layer filter screen mounted on the metal grid. The filter screen is made of polyethylene fiber.

[0049] Furthermore, the first-stage condensing assembly, the second-stage evacuation and diversion assembly, and the third-stage evacuation and diversion assembly are three independent units connected in sequence;

[0050] The first stage condensation assembly includes: a condensation outer shell and a condensation inner tube 600, a closed first cooling channel 601 is formed between the first stage condensation outer shell and the first stage condensation inner tube 600, and a first inlet 603 and a first outlet 607 are opened on the first stage condensation outer shell. The first inlet 630 is connected to the cold water tank 28 through the first flow control valve 282 and the first water inlet pipeline, and the first outlet 607 is connected to the recovery water tank 21 through the second flow control valve 610 and the first return pipeline.

[0051] The replacement speed of the cooling water in the first cooling channel 601 is controlled by setting the opening of the first flow control valve 282 and the second flow control valve 610, so as to control the cooling degree of the steam and the inert gas by the first condensing component;

[0052] The steam passing through the multi-stage composite membrane disposed in the first-stage condensation inner tube 600 is condensed on the mesh during the condensation process. After condensing into water droplets, the water droplets are accelerated to penetrate the multi-stage composite membrane under the action of the inert gas and enter the second-stage gas diversion component. The inert gas freely passes through the multi-stage composite membrane and enters the interior of the second-stage gas diversion component.

[0053] The two-stage air evacuation and diversion assembly includes: a two-stage condensation shell and a two-stage condensation inner tube 604. The two-stage condensation inner tube is configured to have a first groove with a downward inclination at the bottom. The first groove is used to transport condensed water to the three-stage air evacuation and diversion assembly. The upper part of the two-stage condensation inner tube is configured to have a first diversion groove with an upward inclination, and the inert gas is collected into the gas collection tank through the first diversion groove; a first diversion control valve 291 is provided between the first diversion groove and the gas collection tank, and a second cooling channel 605 is formed between the two-stage condensation shell and the two-stage condensation inner tube. A second inlet 606 and a second outlet 608 are provided on the two-stage condensation shell. The second inlet is connected to the cold water tank through the third flow control valve 281 and the second water inlet pipeline, and the second outlet is connected to the recovery water tank through the fourth flow control valve 609 and the second return pipeline; and the replacement speed of the cooling water in the second cooling channel is controlled by setting the opening of the third flow control valve and the fourth flow control valve to achieve the control of the cooling degree of the steam and the inert gas by the two-stage condensation assembly;

[0054] The three-stage gas drainage and diversion assembly includes: a three-stage condensation shell and a three-stage condensation inner tube 616. The three-stage condensation inner tube is configured to have a second groove with a downward slope at the bottom. The second groove is used to transport condensed water to the end of the three-stage condensation inner tube. The upper part of the three-stage condensation inner tube is configured to have a second diversion groove with an upward slope. The inert gas is collected into a gas collection tank through the second diversion groove 617; a second diversion control valve 290 is provided between the second diversion groove 617 and the gas collection tank. A third cooling channel 615 is formed between the three-stage condensation shell and the three-stage condensation inner tube. A third inlet 618 and a third outlet 614 are provided on the three-stage condensation shell. The third inlet is connected to the cold water tank through the fifth flow control valve 280 and the third water inlet pipeline, and the third outlet is connected to the recovery water tank through the sixth flow control valve 613 and the third return pipeline; and the replacement speed of the cooling water in the third cooling channel is controlled by setting the opening of the fifth flow control valve and the sixth flow control valve to achieve the control of the cooling degree of the three-stage condensation assembly on the steam and the inert gas;

[0055] The first groove and the second groove have the same inclination, and the first groove and the second groove are connected at the ends. In the above, the replacement speed of condensed water in the first, second, and third condensing inner tubes decreases successively, that is, the condensation effect of the first condensing inner tube is the best, and the steam can be condensed through the hanging net form. The quality of the condensation effect depends on the heat exchange speed. The present application accelerates the circulation speed of condensed water in the first condensing inner tube, so that the temperature in the first condensing inner tube is maintained at a lower level and the transfer of exchange heat is accelerated.

[0056] The technical principle of the present application is as follows: the control device controls the feed valve 50 to open according to a set period, and feeds a set amount of primary premix into the mixing space 14 from the premix tank, and then controls the feed valve 50 and the return valve 71 to close respectively, and then sets the upper limit value for triggering the pressure control valve 16; the control device controls the pushing cylinder 1 to push the push rod 12 within a set period according to a set set of periodic control instructions to drive the pushing piston 15 to reciprocate in the mixing space 14, and within the set period, the pushing stroke of the pushing piston 15 in the mixing space 14 gradually increases, so that the primary premix in the mixing space 14 is gradually increased during the pushing period. The piston 15 is uniformly mixed during its reciprocating motion, and as the pushing stroke gradually increases, the pressure environment in the mixing space 14 is also gradually increased. The gradual increase in the pressure environment accelerates the mixing of the primary premix. When at the end of the execution of the set cycle, the pushing stroke of the pushing piston 15 gradually reaches the maximum, the pressure in the mixing space 14 reaches the upper limit value triggered by the pressure control valve 16. At this time, the pressure control valve 16 is opened, and the uniformly mixed primary premix forms a reaction material, which is transported to the reaction device 20 under the action of the pushing piston. The uniformly mixed reaction material is dispersed in a fine particle size through the dispersion pipe provided in the reaction device 20. The reaction material is sprayed into the reaction chamber provided in the reaction device 20 in the form of fine particles; when the pressure in the mixing space 14 drops below the upper limit value triggered by the pressure control valve 16, the pressure control valve 16 is closed, and the pressure control valve 16 sends a feedback instruction to the control device. When the control device receives the feedback instruction, the control device controls the feed valve 50 to open again according to the set cycle, and feeds a set amount of primary premix into the mixing space 14 from the premix tank, and then controls the feed valve 50 and the reflux valve 71 to close respectively, and controls the mixing device to complete the control of the control instruction set for the next cycle; the reaction material sprayed in the form of fine particles is sprayed into the reaction chamber provided in the reaction device 20 in the form of fine particles; when the pressure in the mixing space 14 drops below the upper limit value triggered by the pressure control valve 16, the pressure control valve 16 is closed, and the pressure control valve 16 sends a feedback instruction to the control device. When the control device receives the feedback instruction, the control device controls the feed valve 50 to open again according to the set cycle, and feeds a set amount of primary premix into the mixing space 14 from the premix tank, and then controls the feed valve 50 and the reflux valve 71 to close respectively, and controls the mixing device to complete the control of the control instruction set for the next cycle; The upper heating block 204 and the lower heating block 207 provided at the upper and lower ends of the reaction chamber are heated and kept boiling until the reaction material is completely dissolved; during the dissolution process of the reaction material, preheated inert gas is introduced through at least one set of aerators provided at the bottom of the reaction chamber to accelerate the movement of the reaction material in the explosive gas of the inert gas to fully dissolve it. At the same time, the steam formed and the floating inert gas are input into the reflux cooling device 6 through the guide pipe provided at one end of the reaction device 20. The steam is condensed by the reflux cooling device 6 and then input into the liquid collecting tank. At the same time, a drainage groove is formed in the reflux cooling device 6 to recover the inert gas to the gas collection tank;After the reaction materials are sequentially added to the reaction apparatus 20 over multiple set cycles, the reaction chamber temperature is maintained constant and aeration is performed for 30-60 minutes, entering the recrystallization stage. The aerator is then stopped, and the upper heating block 204 and the lower heating block 207 are controlled to cool to 40-50°C at a rate of 2-5°C / min and maintained at 40-50°C until recrystallization is complete. After crystallization is complete, the recrystallized primary product is removed through a discharge port provided at the right bottom of the reaction apparatus 20 and placed in a washing apparatus, where it is washed with excess 2-propanol. After washing, the washing liquid is discharged, and the primary product is then dried in the washing apparatus to obtain medrogestrel.

[0057] Example 2

[0058] The present invention also provides a method for preparing medrogestrel, comprising the following steps:

[0059] Step 1) adding 50 kg of progesterone extract mixed with mesosulfuronone seed crystals and 230 L of diacetone from the first dosing tank 3 and the second dosing tank 4 to the premixing tank 5 through the first metering valve 30 and the second metering valve 40 respectively; then slowly stirring for 5-8 hours through the premixing tank 5;

[0060] Step 2) The control device controls the feed valve 50 to open according to the set cycle, and feeds a set amount of primary premix into the mixing space 14 from the premix tank, then controls the feed valve 50 and the return valve 71 to close respectively, and then sets the triggering upper limit value of the pressure control valve 16; the control device controls the pushing cylinder 1 to push the push rod 12 within the set cycle according to the set periodic control instruction set to drive the pushing piston 15 to reciprocate in the mixing space 14, and within the set cycle, the pushing stroke of the pushing piston 15 in the mixing space 14 gradually increases, so that the primary premix in the mixing space 14 is evenly mixed during the reciprocating motion of the pushing piston 15, and when the pushing stroke gradually increases, the pressure environment in the mixing space 14 is also gradually increased. The gradual increase in the pressure environment accelerates the mixing of the primary premix, and at the end of the execution of the set cycle, the pushing activity When the thrust stroke of the plug 15 gradually reaches the maximum, the pressure in the mixing space 14 reaches the upper limit value triggered by the pressure control valve 16. At this time, the pressure control valve 16 is opened, and the uniformly mixed primary premix forms a reaction material, which is transported to the reaction device 20 under the action of the thrust piston. The uniformly mixed reaction material is sprayed into the reaction chamber provided in the reaction device 20 in the form of fine particles through the dispersion pipe provided in the reaction device 20. When the pressure in the mixing space 14 drops below the upper limit value triggered by the pressure control valve 16, the pressure control valve 16 is closed, and the pressure control valve 16 sends a feedback instruction to the control device. When the control device receives the feedback instruction, the control device controls the feed valve 50 to open again according to the set cycle, and feeds a set amount of primary premix into the mixing space 14 from the premix tank, and then controls the feed valve 50 and the reflux valve 71 to close respectively.

[0061] Step 3) Repeat step 2) to spray the uniformly mixed reaction materials obtained in multiple cycles into the reaction chamber provided in the reaction device 20 in the form of fine particles until all the primary premix is ​​added to the mixing device and transferred from the mixing device to the reaction device 20;

[0062] Step 4) The reaction material sprayed in the form of fine particles is heated and kept boiling in the reaction chamber by the upper heating block 204 and the lower heating block 207 arranged at the upper and lower ends of the reaction chamber until the reaction material is completely dissolved; during the dissolution of the reaction material, preheated inert gas is introduced through at least one set of aerators arranged at the bottom of the reaction chamber to accelerate the movement of the reaction material in the explosive gas of the inert gas to fully dissolve it. At the same time, the steam formed and the floating inert gas are input into the reflux cooling device 6 through the guide pipe provided at one end of the reaction device 20. The steam is condensed by the reflux cooling device 6 and then input into the liquid collecting tank. At the same time, a drainage groove is formed in the reflux cooling device 6 to recover the inert gas to the gas collection tank;

[0063] Step 5) After the reaction materials are sequentially added to the reaction device 20 in multiple set cycles, the reaction chamber temperature is maintained unchanged and the gas is exploded for 30-60 minutes, entering the recrystallization stage, and then the aerator is stopped, and the upper heating block 204 and the lower heating block 207 are controlled to cool to 40-50°C at a rate of 2-5°C / min, and maintained at 40-50°C until the recrystallization is completed. After the crystallization is completed, the recrystallized primary product is taken out through the discharge port provided at the bottom right side of the reaction device 20 and placed in a washing device, and washed with excess 2-propanol in the washing device. After washing, the washing liquid is discharged, and then the primary product is dried in the washing device to obtain medrogestrel.

[0064] After step 3) is completed, the control device controls the reflux valve 71 to open, and the recovered liquid collected in the liquid collecting tank enters the mixing device through the reflux valve 71, the reflux pipeline, and the reflux port 18. The pushing piston 15 is controlled to perform reciprocating motion in the mixing space 14 to mix the recovered liquid evenly again and then input it into the reaction device 20.

[0065] 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, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A preparation device for medrogestrel, characterized in that: include: The premixing tank is used to premix the progesterone extract and dipropylene glycol in a set ratio to form a primary premix; The mixing device is used to add the primary premix in the premix tank in a quantitative manner according to a set period and fully mix it according to a set rule under the control of the control device to form a reaction material; the reaction material is added to the reaction device in batches according to the set period; The reaction device is used to spray the uniformly mixed reaction materials in the form of fine particles into a reaction chamber provided in the reaction device through a dispersion pipe, and then heat and keep boiling by upper and lower heating blocks provided at the upper and lower ends of the reaction chamber until the reaction materials are completely dissolved; during the dissolution of the reaction materials, preheated inert gas is introduced through at least one group of aerators provided at the bottom of the reaction chamber to accelerate the movement of the reaction materials in the aeration of the inert gas to fully dissolve them, and the steam formed and the floating inert gas are input into the reflux cooling device through a guide pipe provided at one end of the reaction device, and the steam is condensed by the reflux cooling device and then input into the liquid collecting tank, and a drainage groove is formed in the reflux cooling device to recover the inert gas to the gas collection tank; After the reaction materials are sequentially added to the reaction device in multiple set cycles, the temperature of the reaction chamber is maintained constant and aeration is continued for 30-60 minutes, then the process enters the recrystallization stage, the aerator is stopped, the upper and lower heating blocks are controlled to cool to 40-50° C. at a rate of 2-5° C. / min, and the temperature is maintained at 40-50° C. until the recrystallization is completed. After the crystallization is completed, the recrystallized primary product is taken out through a discharge port provided at the right bottom of the reaction device and placed in a washing device, washed with excess 2-propanol in the washing device, and the washing liquid is discharged after washing is completed. The primary product is then dried in the washing device to obtain medrogestrel. In which, the mixing device includes a mixing shell, a mixing space is formed inside the mixing shell, and a pushing piston is provided at one end of the left side of the mixing shell, the left side of the pushing piston is connected to the push rod, and the push rod is provided on the pushing cylinder, and a feed port, a discharge port and a reflux port are provided on the mixing shell, a feed valve is provided at the feed port, the premixing tank is connected to the feed valve through a premixing pipeline, and a pressure control valve is provided at the discharge port, and the pressure control valve is connected to the reaction device through a feed pipeline.

2. The preparation device of medrogestrel according to claim 1, characterized in that The premixing tank is connected to the first dosing tank and the second dosing tank respectively.

3. The preparation device of medrogestrel according to claim 1, characterized in that The reaction device includes a reactor shell, an isolation plate arranged on the left side of the reactor shell, a reaction chamber is formed on the right side of the isolation plate and inside the reactor shell, an upper heating block and a lower heating block are respectively arranged at the upper and lower ends of the reaction chamber, and at least one set of aerators is arranged at the bottom of the reaction chamber, the aerators are connected to the preheating tank through an aeration pipeline and an aeration control valve, and the preheating tank is connected to the gas source tank; on the right side of the reaction chamber, a baffle is arranged against the inner wall of the reaction chamber, and a guide is arranged on the upper part of the baffle A guide filter is provided at the guide port, and on the right side of the guide filter is a guide pipe integrated with the reactor shell. A guide channel is formed inside the guide pipe, and a guide plate is provided inside the guide channel, and the guide plate is provided on the right side of the guide filter, and the guide channel is divided into an upper guide groove and a lower ventilation groove by the guide plate. An air increase pipe is provided at the bottom of the guide pipe and located at the lower ventilation groove, and the air increase pipe is connected to the gas source tank through an air increase pipeline; the end of the guide channel is connected to the reflux cooling device.

4. The preparation device of medrogestrel according to claim 1, characterized in that The reflux cooling device is a three-stage cooling device, including a first-stage condensing component in which a multi-stage composite membrane is arranged; a second-stage air drainage guide component connected to the first-stage condensing component and a third-stage air drainage guide component connected to the second-stage air drainage guide component; the ends of the three-stage air drainage guide components are connected to the liquid collecting tank through a guide pipe, and the liquid collecting tank is connected to the reflux port through a reflux pipe and a reflux valve.

5. The preparation device of medrogestrel according to claim 4, characterized in that The first stage condensing assembly, the second stage evacuation and diversion assembly, and the third stage evacuation and diversion assembly are three independent units connected in sequence; The first stage condensing assembly includes: a condensing outer shell and a condensing inner tube, a closed first cooling channel is formed between the condensing outer shell and the condensing inner tube, and a first inlet and a first outlet are opened on the condensing outer shell, the first inlet is connected to the cold water tank through a first flow control valve and a first water inlet pipeline, and the first outlet is connected to the recovery water tank through a second flow control valve and a first return pipeline; The replacement speed of the cooling water in the first cooling channel is controlled by setting the opening of the first flow control valve and the second flow control valve, so as to control the cooling degree of the steam and the inert gas by the first condensing component; The steam passing through the multi-stage composite membrane arranged in the first-stage condensation inner tube is condensed on the mesh during the condensation process. After condensing into water droplets, the water droplets are accelerated to penetrate the multi-stage composite membrane under the action of the inert gas and enter the second-stage gas drainage and diversion component. The inert gas freely passes through the multi-stage composite membrane and enters the interior of the second-stage gas drainage and diversion component. The two-stage air evacuation and diversion assembly includes: a two-stage condensation outer shell and a two-stage condensation inner tube, the two-stage condensation inner tube is configured to have a first groove with a downward inclination at the bottom, the first groove is used to transport condensed water to the three-stage air evacuation and diversion assembly, and the upper part of the two-stage condensation inner tube is configured to have a first diversion groove with an upward inclination, and the inert gas is collected into the gas collection tank through the first diversion groove; a second cooling channel is formed between the two-stage condensation outer shell and the two-stage condensation inner tube, a second inlet and a second outlet are opened on the two-stage condensation outer shell, the second inlet is connected to the cold water tank through a third flow control valve and a second water inlet pipe, and the second outlet is connected to the recovery water tank through a fourth flow control valve and a second return pipe; and the replacement speed of the cooling water in the second cooling channel is controlled by setting the opening of the third flow control valve and the fourth flow control valve, so as to achieve the control of the cooling degree of the steam and the inert gas by the two-stage air evacuation and diversion assembly; The three-stage air evacuation and diversion assembly includes: a three-stage condensation outer shell and a three-stage condensation inner tube, the three-stage condensation inner tube is configured to have a second groove with a downward slope at the bottom, the second groove is used to transport condensed water to the end of the three-stage condensation inner tube, and the upper part of the three-stage condensation inner tube is configured to have a second diversion groove with an upward slope, and the inert gas is collected into the gas collection tank through the second diversion groove; a third cooling channel is formed between the three-stage condensation outer shell and the three-stage condensation inner tube, a third inlet and a third outlet are opened on the three-stage condensation outer shell, the third inlet is connected to the cold water tank through the fifth flow control valve and the third water inlet pipeline, and the third outlet is connected to the recovery water tank through the sixth flow control valve and the third return pipeline; and the replacement speed of the cooling water in the third cooling channel is controlled by setting the opening of the fifth flow control valve and the sixth flow control valve, so as to achieve the control of the cooling degree of the steam and inert gas by the three-stage air evacuation and diversion assembly; The first groove and the second groove have the same inclination, and the first groove and the second groove are connected at the end.

6. The preparation device of medrogestrel according to claim 4, characterized in that The control device controls the feed valve to open according to a set period, and feeds a set amount of primary premix into the mixing space from the premix tank, then controls the feed valve and the return valve to close respectively, and then sets the upper limit value for triggering the pressure control valve; the control device controls the push cylinder to push the push rod within the set period according to the set periodic control instruction set to drive the push piston to reciprocate in the mixing space, and within the set period, the pushing stroke of the push piston in the mixing space gradually increases, so that the primary premix in the mixing space is evenly mixed during the reciprocating motion of the push piston, and when the pushing stroke gradually increases, the pressure environment in the mixing space is also gradually increased, and the gradual increase in the pressure environment accelerates the mixing of the primary premix, and at the end of the execution of the set period, the pushing stroke of the push piston gradually reaches the maximum When the pressure in the mixing space reaches the upper limit value triggered by the pressure control valve, the pressure control valve is opened, and the evenly mixed primary premix forms a reaction material, which is transported to the reaction device under the action of the propulsion piston, and the evenly mixed reaction material is sprayed into the reaction chamber provided in the reaction device in the form of refined particles through the dispersion pipe provided in the reaction device; when the pressure in the mixing space drops below the upper limit value triggered by the pressure control valve, the pressure control valve is closed, and the pressure control valve sends a feedback instruction to the control device. When the control device receives the feedback instruction, the control device controls the feed valve to open again according to the set cycle, and feeds a set amount of primary premix into the mixing space from the premix tank, and then controls the feed valve and the reflux valve to close respectively, and controls the mixing device to complete the control of the control instruction set for the next cycle.

7. The preparation device of medrogestrel according to claim 2, characterized in that The first dosing tank and the second dosing tank are connected to the premixing tank through a first metering valve, a second metering valve and corresponding delivery pipelines, respectively.

8. A method for preparing medrogestrel, comprising the medrogestrel preparation device according to any one of claims 4 and 6, characterized in that: The steps include: Step 1) adding 50 kg of progesterone extract mixed with mesosulfuronone seed crystals and 230 L of diacetone from the first dosing tank and the second dosing tank to the premixing tank through the first metering valve and the second metering valve, respectively; then slowly stirring for 5-8 hours through the premixing tank; Step 2) The control device controls the feed valve to open according to the set cycle, and feeds a set amount of primary premix into the mixing space from the premix tank, then controls the feed valve and the return valve to close respectively, and then sets the upper limit value of the triggering of the pressure control valve; the control device controls the pushing cylinder to push the push rod within the set cycle according to the set periodic control instruction set to drive the pushing piston to reciprocate in the mixing space, and within the set cycle, the pushing stroke of the pushing piston in the mixing space gradually increases, so that the primary premix in the mixing space is evenly mixed during the reciprocating motion of the pushing piston, and when the pushing stroke gradually increases, the pressure environment in the mixing space is also gradually increased. The gradual increase in the pressure environment accelerates the mixing of the primary premix, and at the end of the execution of the set cycle, the pushing cylinder is pushed. When the propulsion stroke of the material piston gradually reaches the maximum, the pressure in the mixing space reaches the upper limit value triggered by the pressure control valve. At this time, the pressure control valve is opened, and the evenly mixed primary premix forms a reaction material, which is transported to the reaction device under the action of the propulsion piston. The evenly mixed reaction material is sprayed into the reaction chamber provided in the reaction device in the form of fine particles through the dispersion pipe provided in the reaction device; when the pressure in the mixing space drops below the upper limit value triggered by the pressure control valve, the pressure control valve is closed, and the pressure control valve sends a feedback instruction to the control device. When the control device receives the feedback instruction, the control device controls the feed valve to open again according to the set cycle, and feeds a set amount of primary premix into the mixing space from the premix tank, and then controls the feed valve and the reflux valve to close respectively; Step 3) Repeat step 2) to spray the uniformly mixed reaction materials obtained in multiple cycles into a reaction chamber provided in the reaction device in the form of fine particles until all the primary premix is ​​added to the mixing device and transferred from the mixing device to the reaction device; Step 4) The reaction material sprayed in the form of fine particles is heated to 180-200° C. in the reaction chamber by upper and lower heating blocks disposed at the upper and lower ends of the reaction chamber and kept boiling until the reaction material is completely dissolved. During the dissolution of the reaction material, preheated inert gas is introduced through at least one set of aerators disposed at the bottom of the reaction chamber to accelerate the movement of the reaction material in the aeration of the inert gas, thereby fully dissolving the reaction material. Simultaneously, the generated vapor and the rising inert gas are input into a reflux cooling device through a guide pipe disposed at one end of the reaction device. The vapor is condensed by the reflux cooling device and then input into a liquid collecting tank. Simultaneously, a drainage groove is formed in the reflux cooling device to recover the inert gas to a gas collection tank. Step 5) After the reaction materials are sequentially added to the reaction device in multiple set cycles, the temperature of the reaction chamber is maintained constant and aeration is continued for 30-60 minutes to enter the recrystallization stage. The aerator is then stopped, and the upper and lower heating blocks are controlled to cool to 40-50°C at a rate of 2-5°C / min and maintained at 40-50°C until recrystallization is completed. After crystallization is completed, the recrystallized primary product is removed through a discharge port provided at the bottom right side of the reaction device and placed in a washing device. The product is washed with excess 2-propanol in the washing device. After washing, the washing liquid is discharged, and the primary product is dried in the washing device to obtain medrogestrel.

9. The method for preparing medrogestrel according to claim 8, wherein After step 3) is completed, the control device controls the reflux valve to open, and the recovered liquid collected in the liquid collecting tank enters the mixing device through the reflux valve, reflux pipeline, and reflux port. The pushing piston is controlled to perform reciprocating motion in the mixing space to uniformly mix the liquid again and then input it into the reaction device.

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