CN115069189B - Reaction device for preparing progesterone - Google Patents
Reaction device for preparing progesterone Download PDFInfo
- Publication number
- CN115069189B CN115069189B CN202210873290.5A CN202210873290A CN115069189B CN 115069189 B CN115069189 B CN 115069189B CN 202210873290 A CN202210873290 A CN 202210873290A CN 115069189 B CN115069189 B CN 115069189B
- Authority
- CN
- China
- Prior art keywords
- pressure
- air flow
- heating
- pipeline
- crystallization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J7/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms
- C07J7/0005—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21
- C07J7/001—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21 substituted in position 20 by a keto group
- C07J7/0015—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21 substituted in position 20 by a keto group not substituted in position 17 alfa
- C07J7/002—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of two carbon atoms not substituted in position 21 substituted in position 20 by a keto group not substituted in position 17 alfa not substituted in position 16
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a reaction device for preparing progesterone, and belongs to the technical field of medicines. The reaction device comprises: a control device and a crystallization reactor; the crystallization reactor is internally provided with a pressure sensor and a plurality of groups of crystallization reaction beds which are staggered from bottom to top, the upper and lower sides of the outside of the crystallization reactor are respectively provided with an upper hot air flow generating device and a lower hot air flow generating device, and the side wall of the crystallization reactor is provided with an exhaust valve component; the control device sets the pressure maintaining pressure during crystallization reaction based on the degree of the crystallization reaction, and sets the initial pressure for triggering the exhaust valve assembly to exhaust based on the pressure maintaining pressure, so as to control the dynamic balance of the internal pressure of the crystallization reactor; the control device controls the upper hot air flow generating device and the lower hot air flow generating device to form high-pressure hot air flow based on initial pressure, and the materials on the crystallization reaction bed are crystallized and grown, so that stirring is not needed, a disordered state of the system is avoided, and crystallization and crystal growth are facilitated.
Description
Technical Field
The invention relates to the technical field of medicines, in particular to a reaction device for preparing progesterone.
Background
Progesterone is a human endogenous progestogen that plays an important role in the human fertility process. Is widely applied to functional uterine bleeding, threatened abortion, habitual abortion, menorrhagia, dysmenorrhea, amenorrhea, endometriosis and advanced breast cancer clinically, and is one of the most basic progestational medicaments.
The progesterone needs crystallization reaction in the production process, the progesterone is stirred by a stirring device in the crystallization reaction of the prior art, and is recrystallized in the production process, because the recrystallization process is the crystal growth process, the most important step in the growth process is the nucleation process, transient fine crystal particles appear everywhere in the system, and the process is not suitable for stirring, stirring or violent vibration, so that the system is in a disordered state, and the formation of crystal lattices is not facilitated.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a reaction device for preparing progesterone. The reaction apparatus includes: a control device and a crystallization reactor;
the crystallization reactor is internally provided with a pressure sensor and a plurality of groups of crystallization reaction beds which are staggered from bottom to top, the upper and lower sides of the outside of the crystallization reactor are respectively provided with an upper hot air flow generating device and a lower hot air flow generating device, and the side wall of the crystallization reactor is provided with an exhaust valve assembly;
an upper pressurizing system is arranged at the top of the outer side of the upper hot air flow generating device, an upper heating system is arranged in the upper hot air flow generating device, a lower pressurizing system is arranged at the bottom of the outer side of the lower hot air flow generating device, and a lower heating system is arranged in the lower hot air flow generating device;
the control device is electrically connected with the pressure sensor, the upper pressurizing system, the upper heating system, the lower pressurizing system and the lower heating system, and is used for setting the pressure maintaining pressure during crystallization reaction based on the degree of crystallization reaction required, and the control device is used for setting the initial pressure triggering the exhaust valve assembly to exhaust based on the pressure maintaining pressure so as to control the dynamic balance of the internal pressure of the crystallization reactor;
the control device is also used for controlling the upper pressurizing system and the lower pressurizing system to form an upper high-pressure air flow and a lower high-pressure air flow in a subsection mode based on the initial pressure, the upper high-pressure air flow and the lower high-pressure air flow are heated by the upper heating system and the lower heating system respectively to form an upper high-pressure hot air flow which is input downwards and a lower high-pressure hot air flow which is input upwards, and the upper high-pressure hot air flow and the lower high-pressure hot air flow enter the crystallization reactor to form thermal convection so as to crystallize and grow crystals on materials on the crystallization reaction bed.
Further, the upper hot air flow generating device includes: an upper housing; an upper fixing plate is fixedly connected to the bottom of the side wall of the upper shell, the upper fixing plate is fixed to the top of the crystallization reactor through an upper fixing component, an upper control valve is arranged at the top of the crystallization reactor, an upper air flow inlet is arranged at the bottom of the upper shell, the upper control valve corresponds to the upper air flow inlet in position,
the upper pressurization system includes: the upper pressurizing device is connected to the outer side of the top of the upper shell, an upper mixing cavity is arranged on the upper pressurizing device, the upper mixing cavity is positioned in the upper shell, a first channel and a second channel which are communicated with each other are arranged on the upper pressurizing device, the first channel and the second channel are communicated with the upper mixing cavity, an upper pressurizing pump is connected on the first channel through an upper pressurizing pipeline, a first electromagnetic valve is connected on the second channel, the first electromagnetic valve is connected with an upper fan through an upper fresh air input pipeline,
the upper heating system includes: at least one group of symmetrical upper heating components connected to the inner wall of the upper shell, wherein the upper heating components are positioned below the upper mixing cavity, an upper heating block is connected to the upper heating components, an upper heating channel is formed between the upper heating components,
the first electromagnetic valve, the upper pressurizing pump, the upper fan, the upper control valve and the upper heating component are all electrically connected with the control device.
Further, the lower hot air flow generating device includes: a lower housing;
the top of the side wall of the lower shell is fixedly connected with a lower fixing plate, the lower fixing plate is fixed at the bottom of the crystallization reactor through a lower fixing component, a lower control valve is arranged at the bottom of the crystallization reactor, a lower air flow inlet is arranged at the top of the lower shell, the lower control valve corresponds to the position of the lower air flow inlet,
the lower pressurization system includes: the lower pressurizing device is connected to the outer side of the bottom of the lower shell, a lower mixing cavity is arranged on the lower pressurizing device, the lower mixing cavity is positioned in the lower shell, a third channel and a fourth channel which are communicated with each other are arranged on the lower pressurizing device, the third channel and the fourth channel are communicated with the lower mixing cavity, a lower pressurizing pump is connected to the third channel through a lower pressurizing pipeline, a second electromagnetic valve is connected to the fourth channel, a lower fan is connected to the second electromagnetic valve through a lower fresh air input pipeline,
the lower heating system includes: at least one group of symmetrical lower heating components connected to the inner wall of the lower shell, wherein the lower heating components are positioned above the lower mixing cavity, the lower heating components are connected with lower heating blocks, a lower heating channel is formed between the lower heating components,
the second electromagnetic valve, the lower pressure pump, the lower fan, the lower control valve and the lower heating component are all electrically connected with the control device.
Further, the exhaust valve assembly includes: a valve body and a pressure valve body;
the side wall of the crystallization reactor is provided with an air flow outlet, an air flow output pipeline is connected in the air flow outlet, a pressure cavity which is arranged in a hollow way is arranged in the pressure valve body, one side of the pressure valve body is connected with the air flow output pipeline,
one side of the valve body is connected with one side of the pressure valve body, which is far away from the air flow output pipeline, the valve body is hollow, an air cylinder is fixed in the valve body, the end part of a push rod of the air cylinder is connected with a shaft lever, the other end of the shaft lever is connected with a film pressure plate, the film pressure plate is positioned in the pressure valve body,
the pressure membrane is fixedly connected with the side wall of the pressure valve body, the pressure cavity is divided into two independent first cavities and second cavities, the first cavities are positioned at one side close to the air flow output pipeline, and the second cavities are positioned at one side close to the valve body;
the cylinder is electrically connected with the control device.
Further, the reaction apparatus further comprises: a heat exchanger;
the crystallization reactor comprises a crystallization reactor, wherein the inner wall of the crystallization reactor is connected with a first heat preservation cavity and a second heat preservation cavity, the side wall of the crystallization reactor is connected with a first communication pipeline and a second communication pipeline, the second communication pipeline is communicated with the first heat preservation cavity, the first communication pipeline is communicated with the second heat preservation cavity, and the second communication pipeline and the first communication pipeline are respectively connected with an outlet of the heat exchanger through a second heat exchange pipeline and a first heat exchange pipeline;
the two sides of the pressure valve body are provided with a first airflow port and a second airflow port, the first airflow port and the second airflow port are positioned between the pressure film and the airflow output pipeline, the first airflow port and the second airflow port are respectively connected with an inlet of the heat exchanger through a first exhaust pipeline and a second exhaust pipeline, and the heat exchanger is electrically connected with the control device.
Further, a first outlet pipeline and a second outlet pipeline are further connected to the side wall of the crystallization reactor, the first outlet pipeline is communicated with the first heat preservation cavity, the second outlet pipeline is communicated with the second heat preservation cavity, and the first outlet pipeline and the second outlet pipeline are respectively connected with the heat exchanger through a first heat return pipeline and a second heat return pipeline.
Further, the inner sides of the first heat preservation cavity and the second heat preservation cavity are respectively provided with a first heat conduction sheet and a second heat conduction sheet,
a first heating body and a second heating body are connected in the crystallization reactor, the first heating body and the second heating body are respectively positioned between two ends of the first heat preservation cavity and the second heat preservation cavity, and heating wires are arranged in the first heating body and the second heating body;
the first heating body and the second heating body are respectively connected with two ends of the first heat conducting fin and the second heat conducting fin through a first heat conducting fin and a second heat conducting fin;
the first heating body and the second heating body are electrically connected with the control device.
Further, an upper filter plate and a lower filter plate are respectively connected to the upper airflow inlet and the lower airflow inlet;
an upper air duct is connected to the upper control valve, and the tail end of the upper air duct is connected with an upper air distribution head;
the lower control valve is connected with a lower air duct, and the tail end of the lower air duct is connected with a lower air distribution head;
the upper gas distribution head and the lower gas distribution head are both positioned in the crystallization reactor.
Further, a sealing door is arranged on the side wall of the crystallization reactor.
Further, a spring is sleeved on the shaft rod and is located between the valve body and the film pressure plate.
The beneficial effects of the invention are as follows: in the invention, a crystallization reactor and a control device are arranged, wherein the top and the bottom of the crystallization reactor are respectively provided with an upper hot air flow generating device and a lower hot air flow generating device, a crystallization reaction bed is arranged in the crystallization reactor, the control device sets the pressure maintaining pressure during crystallization reaction based on the degree of crystallization reaction required, and the initial pressure triggering an exhaust valve assembly to exhaust is set based on the pressure maintaining pressure, so that the dynamic balance of the internal pressure of the crystallization reactor is controlled; the control device controls the upper hot air flow generating device and the lower hot air flow generating device to form upper high-pressure hot air flow and lower high-pressure hot air flow based on initial pressure, the upper high-pressure hot air flow and the lower high-pressure hot air flow enter the crystallization reactor to form heat convection, and materials on the crystallization reaction bed are crystallized and grown, so that stirring is not needed, a disordered state of a system is not caused, and the pressure in the crystallization reactor is in dynamic balance, thereby being more beneficial to crystallization and crystal growth.
In addition, the invention is also provided with a heat exchanger, a first heat preservation cavity and a second heat preservation cavity, the heat exchanger is connected with the exhaust valve assembly, the first heat preservation cavity and the second heat preservation cavity, the high-pressure air flow and the high-pressure steam exhausted by the exhaust valve assembly heat exchange at one side of the heat exchanger and then heat the heat medium, the heated heat medium enters the first heat preservation cavity and the second heat preservation cavity to carry out secondary heating heat preservation on the crystallization reaction bed, and the heat medium flows in the first heat preservation cavity and the second heat preservation cavity to enter the heat exchanger for circulation, so that the crystallization and crystal growth efficiency can be improved, the heat of the high-pressure air flow and the high-pressure steam can be utilized, and the energy is saved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a reaction apparatus for preparing progesterone according to the present invention.
Reference numerals: 100-lower fan; 101-a fresh air input pipeline; 102-a second solenoid valve; 103-a lower pressure pump; 104-a lower pressurization line; 105-a lower pressurizing device; 106-a lower mixing chamber; 107-a lower housing; 108-a lower heating assembly; 109-lower heating block; 110-a lower fixing plate; 111-a lower fixing assembly; 112-lower filter plate; 113-a lower control valve; 114-lower heating channel; 200-feeding a fan; 201-feeding fresh air into a pipeline; 202-a first solenoid valve; 203-an upper pressurizing pump; 204-upper pressurization line; 205-upper pressurizing means; 206-an upper mixing chamber; 207-upper housing; 208-an upper heating assembly; 209-upper heating block; 210-upper fixing plate; 211-upper fixing assembly; 212-filtering plate; 213-upper control valve; 214-upper heating channel; 30-a first airflow port; 31-a first cavity; 32-pressure membrane; 33-a pressure valve body; 34-valve body; 35-cylinder; 36-a shaft lever; 37-springs; 38-a second airflow port; 39-an air flow output line; 400-crystallization reactor; 401-a first insulation cavity; 402-a first thermally conductive sheet; 403-a second communication line; 404-a first outlet line; 405-a first conductive sheet; 406—a first heating body; 407-crystallization reaction bed; 408-lower airway; 409-lower gas distribution head; 410-a second insulating cavity; 411-a second outlet line; 412-a second thermally conductive sheet; 413-upper gas distribution head; 414-upper airway; 415-a first communication line; 416-a second conductive sheet; 417-a second heating body; 418-sealing the door; 500-heat exchanger; 501-a second regenerative pipeline; 502-a first regenerative line; 503-a first exhaust line; 504-a second exhaust line; 505-a first heat exchange line; 506-a second heat exchange pipeline; 600-control device.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the embodiments of the present invention will be described in further detail with reference to the accompanying drawings.
A reaction device for preparing progesterone comprises a control device 600, a crystallization reactor 400 and a heat exchanger 500, wherein a sealing door 418 is arranged on the side wall of the crystallization reactor 400 and is used for taking and placing materials. The crystallization reactor 400 is internally provided with a pressure sensor and a plurality of groups of crystallization reaction beds 407 which are staggered from bottom to top, the top of the crystallization reactor 400 is provided with an upper control valve 213, the upper control valve 213 is connected with an upper air duct 414, the tail end of the upper air duct 414 is connected with an upper air distribution head 413, the bottom of the crystallization reactor 400 is provided with a lower control valve 113, the lower control valve 113 is connected with a lower air duct 408, the tail end of the lower air duct 408 is connected with a lower air distribution head 409, and the upper air distribution head 413 and the lower air distribution head 409 are both positioned in the crystallization reactor 400. The crystallization reactor 400 is provided with an upper hot air flow generating device and a lower hot air flow generating device at the upper and lower sides of the outside, respectively, and the sidewall of the crystallization reactor 400 is provided with an exhaust valve assembly.
The upper hot air flow generating device comprises: the bottom of the side wall of the upper shell 207 is fixedly connected with an upper fixing plate 210, the upper fixing plate 210 is fixed on the top of the crystallization reactor 400 through an upper fixing component 211, an upper air flow inlet is formed in the bottom of the upper shell 207, an upper filter plate 212 is connected in the upper air flow inlet and used for filtering impurities, and an upper control valve 213 corresponds to the upper air flow inlet in position; the top of the outside of the upper hot air flow generating device is provided with an upper pressurizing system, and the upper pressurizing system comprises: the upper pressurizing device 205 is connected to the outer side of the top of the upper shell 207, an upper mixing cavity 206 is arranged on the upper pressurizing device 205, the upper mixing cavity 206 is positioned in the upper shell 207, a first channel and a second channel which are communicated with each other are formed in the upper pressurizing device 205, the first channel and the second channel are communicated with the upper mixing cavity 206, the first channel is connected with an upper pressurizing pump 203 through an upper pressurizing pipeline 204, the second channel is connected with a first electromagnetic valve 202, and the first electromagnetic valve 202 is connected with an upper fan 200 through an upper fresh air input pipeline 201; the interior of the upper hot air flow generating device is provided with an upper heating system, and the upper heating system comprises: at least one symmetrical upper heating assembly 208 is connected to the inner wall of the upper housing 207, the upper heating assembly 208 is located below the upper mixing chamber 206, an upper heating block 209 is connected to the upper heating assembly 208, an upper heating channel 214 is formed between the upper heating assemblies 208, and the first electromagnetic valve 202, the upper booster pump 203, the upper blower 200, the upper control valve 213, the upper heating assembly 208 and the pressure sensor are all electrically connected to the control device 600.
The lower hot air flow generating device comprises: the top of the side wall of the lower shell 107 is fixedly connected with a lower fixed plate 110, the lower fixed plate 110 is fixed at the bottom of the crystallization reactor 400 through a lower fixed assembly 111, a lower control valve 113 is arranged at the bottom of the crystallization reactor 400, a lower air flow inlet is formed in the top of the lower shell 107, a lower filter plate 112 is connected to the lower air flow inlet and is used for filtering impurities, and the lower control valve 113 corresponds to the position of the lower air flow inlet; the bottom outside of lower hot gas flow generation device is provided with down the pressurization system, and lower pressurization system includes: the lower pressurizing device 105 is connected to the outer side of the bottom of the lower shell 107, a lower mixing cavity 106 is arranged on the lower pressurizing device 105, the lower mixing cavity 106 is positioned in the lower shell 107, a third channel and a fourth channel which are communicated with each other are formed in the lower pressurizing device 105, the third channel and the fourth channel are communicated with the lower mixing cavity 106, a lower pressurizing pump 103 is connected to the third channel through a lower pressurizing pipeline 104, a second electromagnetic valve 102 is connected to the fourth channel, and the second electromagnetic valve 102 is connected to a lower fan 100 through a lower fresh air input pipeline 101; the inside of lower hot gas flow generation device is provided with lower heating system, and lower heating system includes: at least one group of symmetrical lower heating components 108 connected to the inner wall of the lower housing 107, the lower heating components 108 are located above the lower mixing cavity 106, the lower heating components 108 are connected with a lower heating block 109, a lower heating channel 114 is formed between the lower heating components 108, and the second electromagnetic valve 102, the lower booster pump 103, the lower fan 100, the lower control valve 113 and the lower heating components 108 are all electrically connected with the control device 600.
The exhaust valve assembly includes: the crystallization reactor comprises a valve body 34 and a pressure valve body 33, wherein an air flow outlet is formed in the side wall of the crystallization reactor 400, an air flow output pipeline 39 is connected in the air flow outlet, a hollow pressure cavity is formed in the pressure valve body 33, one side of the pressure valve body 33 is connected with the air flow output pipeline 39, one side of the valve body 34 is connected to one side, far away from the air flow output pipeline 39, of the pressure valve body 33, the valve body 34 is hollow, an air cylinder 35 is fixed in the valve body, the end part of a push rod of the air cylinder 35 is connected with a shaft lever 36, the other end of the shaft lever 36 is connected with a film pressure plate, the film pressure plate is positioned in the pressure valve body 33, a spring 37 is sleeved on the shaft lever 36 and positioned between the valve body 34 and the film pressure plate, a pressure film 32 is arranged in the film pressure plate, the pressure film 32 is fixedly connected with the side wall of the pressure valve body 33, the pressure cavity is divided into two independent first cavities 31 and second cavities, the first cavities 31 are positioned at one side, near the air flow output pipeline 39, and the second cavities are positioned at one side near the valve body 34; the cylinder 35 is electrically connected to the control device 600.
The two sides of the pressure valve body 33 are provided with a first air flow port 30 and a second air flow port 38, the first air flow port 30 and the second air flow port 38 are positioned between the pressure film 32 and the air flow output pipeline 39, the first air flow port 30 and the second air flow port 38 are respectively connected with an inlet of the heat exchanger 500 through a first air exhaust pipeline 503 and a second air exhaust pipeline 504, a first heat preservation cavity 401 and a second heat preservation cavity 410 are connected to the inner wall of the crystallization reactor 400, a first communication pipeline 415 and a second communication pipeline 403 are connected to the side wall of the crystallization reactor 400, the second communication pipeline 403 is communicated with the first heat preservation cavity 401, the first communication pipeline 415 is communicated with the second heat preservation cavity 410, the second communication pipeline 403 and the first communication pipeline 415 are respectively connected with an outlet of the heat exchanger 500 through a second heat exchange pipeline 506 and a first heat exchange pipeline 505, the first outlet pipeline 404 is also connected with the first heat preservation cavity 401, the second outlet pipeline 411 is communicated with the second heat preservation cavity 410, and the first outlet pipeline 501 and the second heat preservation pipeline 500 are respectively connected with the first heat preservation cavity 410 through the first outlet pipeline 411 and the second heat exchange pipeline 501; the heat exchanger 500 is electrically connected to the control device 600.
The inner sides of the first heat preservation cavity 401 and the second heat preservation cavity 410 are respectively provided with a first heat conducting fin 402 and a second heat conducting fin 412, a first heating body 406 and a second heating body 417 are connected in the crystallization reactor 400, the first heating body 406 and the second heating body 417 are respectively positioned between two ends of the first heat preservation cavity 401 and the second heat preservation cavity 410, and heating wires are arranged in the first heating body 406 and the second heating body 417; the first heating body 406 and the second heating body 417 are connected to both ends of the first heat conductive sheet 402 and the second heat conductive sheet 412 through the first conductive sheet 405 and the second conductive sheet 416, respectively; the first heating body 406 and the second heating body 417 are electrically connected to the control device 600.
The application method of the invention can be as follows: the control device 600 controls the first and second heating bodies 406 and 417 to be turned on, and heat of the first and second heating bodies 406 and 417 is transferred to the first and second heat conductive sheets 402 and 412 through the first and second heat conductive sheets 405 and 416, respectively, and the inside of the crystallization reactor 400 is preheated through the first and second heat conductive sheets 402 and 412, and after a period of preheating, the first and second heating bodies 406 and 417 are turned off. Placing the material on the crystallization reaction bed 407, setting a holding pressure (holding pressure is helpful for crystal growth and crystallization) at the time of crystallization reaction by the control device 600 based on the degree of crystallization reaction required, setting an initial pressure for triggering the exhaust valve assembly to exhaust based on the holding pressure, thereby controlling dynamic balance of internal pressure of the crystallization reactor 400, controlling the upper pressurizing system and the lower pressurizing system to form an upper high-pressure air flow and a lower high-pressure air flow based on the initial pressure by the control device 600, controlling output power of the lower pressurizing pump 103 and the upper pressurizing pump 203 based on the initial pressure by the control device 600, respectively, controlling input pressure of fresh air input into the lower pressurizing device 105 and the upper pressurizing device 205 by the lower fan 100 and the upper fan 200 via the second electromagnetic valve 102 and the first electromagnetic valve 202, respectively, obtaining a pressurizing coefficient range of the fresh air in the lower mixing chamber 106 and the upper mixing chamber 206 based on the input pressure, based on the range of the pressurizing coefficient, the fresh air is respectively input to the bottoms of the lower shell and the upper shell after reaching the set input pressure in the lower mixing cavity 106 and the upper mixing cavity 206 to form a lower high-pressure air flow and an upper high-pressure air flow, the lower high-pressure air flow and the upper high-pressure air flow are respectively heated by the lower heating component 108 and the upper heating component 208 through the lower heating channel 114 and the upper heating channel 214 to form a lower high-pressure hot air flow and an upper high-pressure hot air flow, when the crystallization reaction is performed, the control device 600 controls the upper control valve 213 and the lower control valve 113 to be opened and closed simultaneously according to the set period so as to control the lower high-pressure air flow and the upper high-pressure air flow which enter the upper side and the lower side of the crystallization reactor 400 to form heat convection in the crystallization reactor 400, and the heat convection is favorable for crystal growth in the crystallization process and nucleation efficiency is improved.
The pressure balance inside the crystallization reactor is broken by the input lower high pressure gas flow and upper high pressure gas flow and high pressure steam generated in the crystallization reaction inside the crystallization reactor 400, and the control device 600 adjusts the discharge amount of the high pressure hot gas flow and the high pressure steam by controlling the moving distance of the film pressure plate at the vent valve assembly to control the degree of the gas flow outlet (the size of the gas flow outlet being opened) so as to control the dynamic balance of the pressure inside the crystallization reactor 400; when the film pressure plate is pulled upwards by the shaft rod 36 under the action of the air cylinder 35, the air flow outlet is opened, the high-pressure hot air flow and the high-pressure steam exchange heat at one side of the heat exchanger through the first air flow port 30 and the second air flow port 38 by the first air exhaust pipeline 503 and the second air exhaust pipeline 504, then heat the heat medium, the heated heat medium enters the first heat preservation cavity 401 and the second heat preservation cavity 410 through the second heat exchange pipeline 506 and the first heat exchange pipeline 505 respectively, the first heat preservation cavity 401 and the second heat preservation cavity 410 perform secondary heating heat preservation on the crystallization reaction bed 407, the heat medium flows in the first heat preservation cavity 401 and the second heat preservation cavity 410, and the heat medium enters the heat exchanger through the first heat return pipeline 502 and the second heat return pipeline 501 respectively to circulate.
The control device 600 sets an initial pressure by the following method, the control device 600 controls the air cylinder 35 to push the shaft lever 36 to drive the film pressure plate on the shaft lever to move to one side of the air flow output pipeline until a sealing state is formed, and an initial threshold value of the film pressure plate is obtained through conversion according to the pushing stroke of the air cylinder 35 (for example, when in an initial position, a push rod of the air cylinder is in a contracted state, the distance between the film pressure plate and the air flow outlet is the largest, and the air flow outlet is in a fully opened state); setting the opening degree of the air flow outlet through a unit amount of pushing travel, acquiring a set pressure value range corresponding to the opening degree of different air flow outlets through the opening degree of the air flow outlet, storing the set pressure value range corresponding to the opening degree of different air flow outlets in a memory of the control device 600, and simultaneously controlling the back-off process of the air cylinder by the control device 600 according to the set pressure value range corresponding to the opening degree of different air flow outlets, wherein the control device 600 loads stored data in the memory and compares the stored data according to the real-time pressure acquired by the pressure sensor, and when the real-time pressure in the crystallization reactor 400 corresponds to any set pressure value range in the stored data, controlling the air cylinder by the control device 600 according to a preset scheme corresponding to the set pressure value range to back off the film pressure plate; when the real-time pressure is smaller than any set pressure value range, the control device controls the air cylinder to push so as to seal the air flow outlet, that is, the film pressure plate can open the air flow outlet along with the return of the air cylinder only when the real-time pressure is larger than any set pressure value range.
In addition, the holding pressure is different in different stages, a plurality of holding pressures can be set, and the holding pressure is controlled by setting the duration time of each holding pressure; the openings of the air outlets corresponding to different holding pressures are different, and the air outlets can be specifically adjusted by referring to the method.
It is worth to say that in the invention, a crystallization reactor and a control device are provided, wherein the top and the bottom of the crystallization reactor are respectively provided with an upper hot air flow generating device and a lower hot air flow generating device, a crystallization reaction bed is arranged in the crystallization reactor, the control device sets the pressure maintaining pressure during crystallization reaction based on the degree of the needed crystallization reaction, and the initial pressure triggering an exhaust valve assembly to exhaust is set based on the pressure maintaining pressure, so that the dynamic balance of the internal pressure of the crystallization reactor is controlled; the control device controls the upper hot air flow generating device and the lower hot air flow generating device to form upper high-pressure hot air flow and lower high-pressure hot air flow based on initial pressure, the upper high-pressure hot air flow and the lower high-pressure hot air flow enter the crystallization reactor to form heat convection, and materials on the crystallization reaction bed are crystallized and grown, so that stirring is not needed, a disordered state of a system is not caused, and the pressure in the crystallization reactor is in dynamic balance, thereby being more beneficial to crystallization and crystal growth.
In addition, the invention is also provided with a heat exchanger, a first heat preservation cavity and a second heat preservation cavity, the heat exchanger is connected with the exhaust valve assembly, the first heat preservation cavity and the second heat preservation cavity, the high-pressure air flow and the high-pressure steam exhausted by the exhaust valve assembly heat exchange at one side of the heat exchanger and then heat the heat medium, the heated heat medium enters the first heat preservation cavity and the second heat preservation cavity to carry out secondary heating heat preservation on the crystallization reaction bed, and the heat medium flows in the first heat preservation cavity and the second heat preservation cavity to enter the heat exchanger for circulation, so that the crystallization and crystal growth efficiency can be improved, the heat of the high-pressure air flow and the high-pressure steam can be utilized, and the energy is saved.
The foregoing embodiment numbers of the present invention are merely for the purpose of description, and do not represent the advantages or disadvantages of the embodiments.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A reaction device for the preparation of progesterone, characterized in that it comprises: a control device (600) and a crystallization reactor (400);
the crystallization reactor (400) is internally provided with a pressure sensor and a plurality of groups of crystallization reaction beds (407) which are staggered from bottom to top, the upper and lower sides of the outside of the crystallization reactor (400) are respectively provided with an upper hot air flow generating device and a lower hot air flow generating device, and the side wall of the crystallization reactor (400) is provided with an exhaust valve assembly;
an upper pressurizing system is arranged at the top of the outer side of the upper hot air flow generating device, an upper heating system is arranged in the upper hot air flow generating device, a lower pressurizing system is arranged at the bottom of the outer side of the lower hot air flow generating device, and a lower heating system is arranged in the lower hot air flow generating device;
the control device (600) is electrically connected with the pressure sensor, the upper pressurizing system, the upper heating system, the lower pressurizing system and the lower heating system, and is used for setting the pressure maintaining pressure during crystallization reaction based on the degree of crystallization reaction required, and the control device (600) is used for setting the initial pressure triggering the exhaust valve assembly to exhaust based on the pressure maintaining pressure so as to control the dynamic balance of the internal pressure of the crystallization reactor (400);
the control device is further used for controlling the upper pressurizing system and the lower pressurizing system to form an upper high-pressure air flow and a lower high-pressure air flow in a subsection mode based on the initial pressure, the upper high-pressure air flow and the lower high-pressure air flow are heated through the upper heating system and the lower heating system respectively to form an upper high-pressure hot air flow which is input downwards and a lower high-pressure hot air flow which is input upwards, and the upper high-pressure hot air flow and the lower high-pressure hot air flow enter the crystallization reactor (400) to form a heat convection so as to crystallize and grow crystals of materials on the crystallization reaction bed (407).
2. A reaction apparatus for the production of progesterone according to claim 1 wherein the upper hot gas stream generating means comprises: an upper case (207);
an upper fixing plate (210) is fixedly connected to the bottom of the side wall of the upper shell (207), the upper fixing plate (210) is fixed to the top of the crystallization reactor (400) through an upper fixing component (211), an upper control valve (213) is arranged at the top of the crystallization reactor (400), an upper air flow inlet is formed in the bottom of the upper shell (207), the upper control valve (213) corresponds to the upper air flow inlet in position,
the upper pressurization system includes: the upper pressurizing device (205), the upper pressurizing device (205) is connected to the outer side of the top of the upper shell (207), an upper mixing cavity (206) is arranged on the upper pressurizing device (205), the upper mixing cavity (206) is positioned in the upper shell (207), a first channel and a second channel which are communicated are arranged on the upper pressurizing device (205), the first channel and the second channel are communicated with the upper mixing cavity (206), an upper pressurizing pump (203) is connected on the first channel through an upper pressurizing pipeline (204), a first electromagnetic valve (202) is connected on the second channel, an upper fan (200) is connected on the first electromagnetic valve (202) through an upper fresh air input pipeline (201),
the upper heating system includes: at least one group of symmetrical upper heating components (208) connected to the inner wall of the upper shell (207), wherein the upper heating components (208) are positioned below the upper mixing cavity (206), upper heating blocks (209) are connected to the upper heating components (208), an upper heating channel (214) is formed between the upper heating components (208),
the first electromagnetic valve (202), the upper pressurizing pump (203), the upper fan (200), the upper control valve (213) and the upper heating assembly (208) are all electrically connected with the control device (600).
3. A reaction apparatus for the production of progesterone according to claim 2 wherein the lower hot gas stream generating means comprises: a lower case (107);
the top of the side wall of the lower shell (107) is fixedly connected with a lower fixing plate (110), the lower fixing plate (110) is fixed at the bottom of the crystallization reactor (400) through a lower fixing component (111), a lower control valve (113) is arranged at the bottom of the crystallization reactor (400), a lower air flow inlet is arranged at the top of the lower shell (107), the lower control valve (113) corresponds to the position of the lower air flow inlet,
the lower pressurization system includes: the lower pressurizing device (105), the lower pressurizing device (105) is connected to the outer side of the bottom of the lower shell (107), a lower mixing cavity (106) is arranged on the lower pressurizing device (105), the lower mixing cavity (106) is positioned inside the lower shell (107), a third channel and a fourth channel which are communicated with each other are arranged on the lower pressurizing device (105), the third channel and the fourth channel are communicated with the lower mixing cavity (106), a lower pressurizing pump (103) is connected on the third channel through a lower pressurizing pipeline (104), a second electromagnetic valve (102) is connected on the fourth channel, a lower fan (100) is connected on the second electromagnetic valve (102) through a lower fresh air input pipeline (101),
the lower heating system includes: at least one group of symmetrical lower heating assemblies (108) connected to the inner wall of the lower shell (107), wherein the lower heating assemblies (108) are positioned above the lower mixing cavity (106), lower heating blocks (109) are connected to the lower heating assemblies (108), a lower heating channel (114) is formed between the lower heating assemblies (108),
the second electromagnetic valve (102), the lower pressure pump (103), the lower fan (100), the lower control valve (113) and the lower heating assembly (108) are all electrically connected with the control device (600).
4. A reaction apparatus for the preparation of progesterone according to claim 1 wherein the vent valve assembly comprises: a valve body (34) and a pressure valve body (33);
the side wall of the crystallization reactor (400) is provided with an air flow outlet, the air flow outlet is internally connected with an air flow output pipeline (39), the inside of the pressure valve body (33) is a hollow pressure cavity, one side of the pressure valve body (33) is connected with the air flow output pipeline (39),
one side of the valve body (34) is connected with one side of the pressure valve body (33) far away from the airflow output pipeline (39), the valve body (34) is hollow, an air cylinder (35) is fixed in the valve body, the end part of a push rod of the air cylinder (35) is connected with a shaft lever (36), the other end of the shaft lever (36) is connected with a film pressure plate, the film pressure plate is positioned in the pressure valve body (33),
a pressure film (32) is arranged in the film pressure plate, the pressure film (32) is fixedly connected with the side wall of the pressure valve body (33) to divide the pressure cavity into two independent first cavities (31) and second cavities, the first cavities (31) are positioned at one side close to the air flow output pipeline (39), and the second cavities are positioned at one side close to the valve body (34);
the cylinder (35) is electrically connected to the control device (600).
5. The reaction device for the preparation of progesterone according to claim 4, characterized in that it further comprises: a heat exchanger (500);
a first heat preservation cavity (401) and a second heat preservation cavity (410) are connected to the inner wall of the crystallization reactor (400), a first communication pipeline (415) and a second communication pipeline (403) are connected to the side wall of the crystallization reactor (400), the second communication pipeline (403) is communicated with the first heat preservation cavity (401), the first communication pipeline (415) is communicated with the second heat preservation cavity (410), and the second communication pipeline (403) and the first communication pipeline (415) are respectively connected with an outlet of the heat exchanger (500) through a second heat exchange pipeline (506) and a first heat exchange pipeline (505);
the two sides of the pressure valve body (33) are provided with a first air flow port (30) and a second air flow port (38), the first air flow port (30) and the second air flow port (38) are positioned between the pressure film (32) and the air flow output pipeline (39), the first air flow port (30) and the second air flow port (38) are respectively connected with an inlet of the heat exchanger (500) through a first exhaust pipeline (503) and a second exhaust pipeline (504), and the heat exchanger (500) is electrically connected with the control device (600).
6. The reaction device for preparing progesterone according to claim 5, wherein a first outlet pipeline (404) and a second outlet pipeline (411) are further connected to the side wall of the crystallization reactor (400), the first outlet pipeline (404) is communicated with the first heat-preserving cavity (401), the second outlet pipeline (411) is communicated with the second heat-preserving cavity (410), and the first outlet pipeline (404) and the second outlet pipeline (411) are respectively connected with the inlet of the heat exchanger (500) through a first heat-returning pipeline (502) and a second heat-returning pipeline (501).
7. A reaction device for the preparation of progesterone according to claim 5, characterized in that the inner sides of the first (401) and second (410) insulating cavities are provided with a first (402) and a second (412) heat conducting fin, respectively,
a first heating body (406) and a second heating body (417) are connected in the crystallization reactor (400), the first heating body (406) and the second heating body (417) are respectively positioned between two ends of the first heat preservation cavity (401) and the second heat preservation cavity (410), and heating wires are arranged in the first heating body (406) and the second heating body (417);
the first heating body (406) and the second heating body (417) are respectively connected with two ends of the first heat conducting fin (402) and the second heat conducting fin (412) through a first heat conducting fin (405) and a second heat conducting fin (416);
the first heating body (406) and the second heating body (417) are electrically connected with the control device (600).
8. A reaction device for the preparation of progesterone according to claim 3, characterized in that,
an upper filter plate (212) and a lower filter plate (112) are respectively connected to the upper airflow inlet and the lower airflow inlet;
an upper air duct (414) is connected to the upper control valve (213), and the tail end of the upper air duct (414) is connected with an upper air distribution head (413);
the lower control valve (113) is connected with a lower air duct (408), and the tail end of the lower air duct (408) is connected with a lower air distribution head (409);
the upper gas distribution head (413) and the lower gas distribution head (409) are both positioned in the crystallization reactor (400).
9. A reaction device for the preparation of progesterone according to claim 1, characterized in that the crystallization reactor (400) is provided with a sealing door (418) on the side wall.
10. A reaction device for the preparation of progesterone according to claim 4, characterized in that the shaft (36) is sheathed with a spring (37), the spring (37) being located between the valve body (34) and the membrane pressure plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210873290.5A CN115069189B (en) | 2022-07-23 | 2022-07-23 | Reaction device for preparing progesterone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210873290.5A CN115069189B (en) | 2022-07-23 | 2022-07-23 | Reaction device for preparing progesterone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115069189A CN115069189A (en) | 2022-09-20 |
| CN115069189B true CN115069189B (en) | 2023-04-25 |
Family
ID=83243409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210873290.5A Active CN115069189B (en) | 2022-07-23 | 2022-07-23 | Reaction device for preparing progesterone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115069189B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115164532B (en) * | 2022-07-23 | 2023-04-07 | 西安国康瑞金制药有限公司 | Drying device based on progesterone purification usefulness |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN212467187U (en) * | 2020-04-13 | 2021-02-05 | 湖北丹澳药业有限公司 | Pregnenolone's recrystallization device |
Family Cites Families (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2143621Y (en) * | 1992-12-30 | 1993-10-13 | 梁甲学 | Preheating convection device |
| CN1162299A (en) * | 1994-12-22 | 1997-10-15 | 桑特拉德有限公司 | Chemicals crystallisation process |
| WO2004083498A1 (en) * | 2003-03-17 | 2004-09-30 | Osaka Industrial Promotion Organization | Method for producing group iii nitride single crystal and apparatus used therefor |
| JP5415678B2 (en) * | 2007-07-25 | 2014-02-12 | 月島機械株式会社 | Gas lift crystallization apparatus and crystallization method |
| CN201379985Y (en) * | 2009-03-27 | 2010-01-13 | 山东福田药业有限公司 | Sugar alcohol hang drum circulatory evaporative crystallization device |
| KR100924236B1 (en) * | 2009-06-23 | 2009-10-29 | 충남대학교산학협력단 | Methods and apparatus for preparing ultra-fine particles with narrow particle size distribution |
| CN202237356U (en) * | 2011-07-22 | 2012-05-30 | 梁甲学 | Stirring fast sugar boiling convector |
| CN203736892U (en) * | 2014-01-26 | 2014-07-30 | 武汉三联节能环保工程有限公司 | Ammonium sulfate heater and crystallization device combined structure for desulfurization by sintering flue gas ammonia method |
| CN205461107U (en) * | 2016-03-10 | 2016-08-17 | 西华大学 | Reactive crystallization jar for crystallization |
| CN205672600U (en) * | 2016-04-29 | 2016-11-09 | 广西吉然科技有限公司 | A kind of crystallizer jet forced circulation device |
| CN106669581A (en) * | 2017-01-05 | 2017-05-17 | 中国石油天然气集团公司 | Stirring-free reactor, stirring-free PTA curing crystallizing device and technical method thereof |
| CN110285254B (en) * | 2019-07-04 | 2020-05-15 | 惟精环境科技有限公司 | Pneumatic valve positioner and control method thereof |
| CN213433060U (en) * | 2020-09-07 | 2021-06-15 | 广州德程机电设备有限公司 | Controllable crystallizer |
| CN112552166A (en) * | 2020-12-10 | 2021-03-26 | 浙江中控技术股份有限公司 | Oleic acid crystallization process control method and device |
| CN113956318A (en) * | 2021-09-10 | 2022-01-21 | 丽江映华生物药业有限公司 | Progesterone refining method |
| CN114380879A (en) * | 2022-01-26 | 2022-04-22 | 成都倍特药业股份有限公司 | Method for preparing progesterone intermediate and progesterone by using microchannel reactor |
-
2022
- 2022-07-23 CN CN202210873290.5A patent/CN115069189B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN212467187U (en) * | 2020-04-13 | 2021-02-05 | 湖北丹澳药业有限公司 | Pregnenolone's recrystallization device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115069189A (en) | 2022-09-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN115069189B (en) | Reaction device for preparing progesterone | |
| CN109081563A (en) | 3D glass heat bender and 3D glass forming method | |
| CN207842069U (en) | A kind of cast type 3D printer | |
| CN201653128U (en) | Heating batching out unit of soft ferrite sintering kiln | |
| CN115164532B (en) | Drying device based on progesterone purification usefulness | |
| US3609296A (en) | Electrically heated autoclave apparatus | |
| CN112548959B (en) | Double-shaft temperature control rotary table and temperature control system thereof | |
| JPH11186015A (en) | Manufacturing equipment of rare-earth magnet powder | |
| CN207770834U (en) | One kind is powder metallurgy sintered to use close furnace | |
| CN112275246B (en) | Thermal cycle chemical industry reation kettle | |
| CN204348848U (en) | A kind of hot air circulating system of lead-acid battery curing room | |
| CN209706546U (en) | A kind of FERRITE CORE hot air circulation sintering system | |
| CN208887262U (en) | Vacuum box equipment | |
| CN203112811U (en) | Three-dimensional structure shaping chamber for cell | |
| CN114671773A (en) | High-yield cyclic acid synthesis method | |
| CN208580805U (en) | The thermal control system of pile | |
| CN213578648U (en) | Pseudo-boehmite stoving dust collection overheat protection device | |
| CN106637015A (en) | Heat treatment technology for refining Ti-5Al-2.5Sn ELI alloy casting structure | |
| CN221403921U (en) | Box-type furnace for sintering battery anode material | |
| CN115954505B (en) | Method for cold start of fuel cell stack | |
| CN219956093U (en) | Uniform heating auxiliary device for electronic sintering furnace | |
| CN214715739U (en) | A carbomorphism device for carbon film preparation | |
| CN212962493U (en) | Drying cabinet that mutual-inductor solidification was used | |
| CN109556409A (en) | A kind of high temp sintering device and its sintering process method of Fast Sintering | |
| CN222012702U (en) | Sintering device of composite ceramic fiber module |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |