CN115178213A - Preparation system and preparation process of dexamethasone sodium phosphate - Google Patents
Preparation system and preparation process of dexamethasone sodium phosphate Download PDFInfo
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- CN115178213A CN115178213A CN202210815068.XA CN202210815068A CN115178213A CN 115178213 A CN115178213 A CN 115178213A CN 202210815068 A CN202210815068 A CN 202210815068A CN 115178213 A CN115178213 A CN 115178213A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/02—Crystallisation from solutions
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Abstract
The invention belongs to the technical field of crystallization, and particularly discloses a preparation system of dexamethasone sodium phosphate, which comprises a condition control system, a reaction tank assembly and a crystallization assembly; the condition control system is connected with the reaction tank assembly and at least used for providing low-temperature conditions and heat preservation conditions required by reaction for the reaction tank assembly; the crystallization assembly is communicated with the reaction tank body through a pipeline and is used for conveying a reaction product of the reaction tank assembly to the crystallization assembly for crystallization. According to the invention, through multi-stage standing and phase splitting, the water phase and the oil phase are separated thoroughly, the product precision of dexamethasone sodium phosphate is improved, crystal growth is formed through the heat convection of the upper heating block and the lower heating block in the crystallization process, the crystal quality is improved, and the dexamethasone sodium phosphate is convenient to store.
Description
Technical Field
The invention belongs to the technical field of crystallization, and particularly relates to a preparation system and a preparation process of dexamethasone sodium phosphate.
Background
Dexamethasone sodium phosphate, chemical name of which is 16 alpha-methyl-11 beta, 17 alpha, 21 trihydroxy-9 alpha-fluoropregna-1,4-diene-3,20-diketone-21-phosphate disodium salt, is an adrenocortical hormone medicament, and has the functions of resisting inflammation, resisting allergy, resisting rheumatism and immunosuppression.
In the prior art, dexamethasone sodium phosphate is mostly stored in a crystal state, but the crystal state and crystallization conditions are not researched, so that the heat resistance of the dexamethasone sodium phosphate is poor, the dexamethasone sodium phosphate is not easy to store, and in the preparation process of the dexamethasone sodium phosphate, the separation of a water phase and an oil phase is incomplete, so that the product precision is poor.
Therefore, it is a technical problem to be solved by those skilled in the art to provide a novel preparation system and process for dexamethasone sodium phosphate.
Disclosure of Invention
The invention aims to overcome the defects of poor accuracy and poor storage of dexamethasone sodium phosphate in the prior art, and provides a preparation system of dexamethasone sodium phosphate.
The invention provides a preparation system of dexamethasone sodium phosphate, which comprises a condition control system, a reaction tank component and a crystallization component, wherein the reaction tank component comprises a reaction tank and a crystallization component;
the condition control system is connected with the reaction tank assembly and at least used for providing low-temperature conditions and heat preservation conditions required by the reaction to the reaction tank assembly;
the crystallization component is communicated with the reaction tank body through a pipeline and is used for conveying a reaction product of the reaction tank component to the crystallization component for crystallization;
the reaction tank assembly includes: the tank body is arranged on the support;
the jar body includes: the reaction tank, the upper cover and the isolation tank body;
the outside of the reaction tank is provided with a conduction sheet, the outside of the conduction sheet is provided with a sealed temperature control area formed around the circumference of the reaction tank, and the outside of the temperature control area is the inner wall of the tank body; a first inlet is formed in one side of the temperature control area, the first inlet extends to the outside of the reaction tank, a first switch valve is arranged at the first inlet, a first outlet is formed in the other side of the temperature control area, the first outlet extends to the outside of the reaction tank, and a second switch valve is arranged at the first outlet;
a stirring device is arranged in the reaction tank;
the upper cover is positioned at the top of the reaction tank, and is provided with a first feed inlet, a second feed inlet, a third feed inlet and a fourth feed inlet which are communicated with the reaction tank respectively;
the isolation tank body is positioned at the bottom of the reaction tank, the bottom of the isolation tank body is sealed, the isolation tank body is hollow, the interior of the isolation tank body is divided into six functional areas from top to bottom, the first functional area is a first standing tank, the second functional area is a first water collecting tank and a first oil phase tank which are arranged side by side, the third functional area is a second standing tank, the fourth functional area is a second oil phase tank and a second water collecting tank which are arranged side by side, the fifth functional area is an activated carbon filter layer, and the sixth functional area is a collection tank;
one side of the first water collecting tank is connected to the water collecting tank through a third outlet and a thirteenth switch valve;
a fifth feeding port is formed in the tank body shell on one side of the upper part of the second standing tank, a seventh switch valve is arranged at the fifth feeding port, and the seventh switch valve is connected with the condition control system through a pipeline;
a fourth outlet is formed in one side of the second oil phase tank and connected to the oil phase tank through a fourteenth switching valve;
a second outlet is formed in the collecting tank, an eleventh switch valve is arranged at the second outlet, and the second outlet is connected to the multistage mesh membrane filter through the eleventh switch valve;
the multistage web filter is in communication with the crystallization assembly.
The reaction tank is characterized in that a third switch valve is arranged at the bottom of the reaction tank and connected to a first standing tank through a first standing input pipeline;
a fourth switch valve and a fifth switch valve are arranged at the bottom of the first standing tank, the fourth switch valve is connected to the first water collecting tank through a pipeline, and the fifth switch valve is connected to the first oil phase tank through a pipeline;
a sixth switching valve is arranged at the bottom of the first oil phase tank and connected to the second standing tank through a pipeline;
an eighth switch valve and a ninth switch valve are arranged at the bottom of the second standing tank, the eighth switch valve is connected to the second oil phase tank through a pipeline, and the ninth switch valve is connected to the second water collecting tank through a pipeline;
the bottom of the second water collecting tank is provided with a tenth switch valve, the tenth switch valve is connected to the activated carbon filtering layer, and the bottom of the activated carbon filtering layer is provided with a filtering plate.
A lining plate is arranged on the inner wall of the isolation tank body, a first support plate is arranged between the first functional area and the second functional area, and two sides of the first support plate are fixed on the lining plate;
a second support plate is arranged between the second functional area and the third functional area, and two sides of the second support plate are fixed on the inner lining plate;
a third support plate is arranged between the third functional area and the fourth functional area, and two sides of the third support plate are fixed on the inner lining plate;
a fourth supporting plate is arranged between the fourth functional area and the fifth functional area, and two sides of the fourth supporting plate are fixed on the inner lining plate.
The condition control system comprises an electric cabinet, wherein an isolation substrate is arranged at the upper part of the electric cabinet, a cold storage box is arranged at the upper part of the isolation substrate, and a base is arranged at the upper part of the cold storage box;
a heating fan is arranged on one side of the top of the base; a supporting seat is arranged in the middle of the top of the base, a refrigerating unit is arranged on the upper portion of the supporting seat, and the refrigerating unit is connected to the cold storage box through a refrigerating pipeline and an electromagnetic valve; a sodium hydroxide solution tank is arranged on the other side of the top of the base;
the feeding pipeline of the sodium hydroxide solution tank is communicated with the seventh switch valve;
the cold accumulator is communicated with the first switch valve through a cold gas pipe and a first interface of a first two-way valve;
the heating fan is communicated with a second interface of the first two-way valve through a hot air pipeline;
the cold accumulator is communicated with the second switch valve through a return pipeline and a first interface of a second two-way valve, and a second interface of the second two-way valve is communicated with the outside of the reaction tank.
The further scheme is that the crystallization assembly comprises a crystallization tank and an acetone storage tank;
a recovery opening is formed in one side of the top of the crystallization tank, a nozzle is arranged in the center of the top of the crystallization tank, a pressurizing device is arranged at the top of the nozzle, and a pressurizing pipe is arranged on one side of the pressurizing device; a discharge port is formed in the bottom of the crystallization tank and connected to a crystal collecting tank through a pipeline and a fifteenth switch valve;
the multistage omentum filter is communicated with a first interface of a three-way valve through a water phase solution pipeline, the acetone storage tank is communicated with a second interface of the three-way valve through a pipeline and a sixteenth switch valve, and a third interface of the three-way valve is communicated with the pressurizing device through a mixer and a twelfth switch valve;
the crystallizer top is provided with the heating piece, and the crystallizer bottom is provided with down the heating piece, go up the heating piece and all be provided with the heater strip down with heating piece inside.
The top of the recovery port is provided with an exhaust valve assembly;
the exhaust valve assembly comprises a valve body and a stroke seat, one end of the valve body is butted with the recovery port, and the stroke seat is arranged at the upper part of the valve body;
a film pressure plate is arranged in the valve body, a film transversely penetrating through the film pressure plate is embedded in the film pressure plate, and two sides of the film are fixed on fixing lugs in the valve body;
the upper part of the film pressure plate is provided with a shaft rod, a spring is arranged outside the shaft rod, the spring is clamped at the joint of the stroke seat and the valve body, a sealing seat is arranged between the stroke seat and the valve body, and the shaft rod penetrates through the sealing seat.
The further scheme is that a temperature controller is arranged on one side of the crystallizing tank and used for controlling the temperature of the heating wire.
The further proposal is that the first to sixteenth switch valves are respectively connected with a control device in the electric cabinet;
and metering pumps are respectively arranged at the first feeding port, the second feeding port, the third feeding port, the fourth feeding port and the fifth feeding port.
The second aspect of the invention provides a preparation process of dexamethasone sodium phosphate, wherein the preparation process adopts the preparation system, and the preparation process comprises the following steps:
step 1, preparing a dexamethasone phosphate solution:
adding anhydrous tetrahydrofuran into the reaction tank through the first feeding port, adding dexamethasone into the reaction tank through the second feeding port, stirring, controlling the opening of the first two-way valve to enable cold airflow at-70 ℃ in the cold accumulator to enter the temperature control area, enabling the temperature inside the reaction tank to be reduced to-55 ℃, adding pyrophosphate chloride into the reaction tank, and stirring; adding pure water for hydrolysis, discharging cold air in the reaction tank, closing an electromagnetic valve on a return pipeline when the cold air is discharged by more than 70%, sending hot air to a temperature control area by a heating fan, simultaneously keeping a second switch valve open, gradually heating the reaction tank to 25-30 ℃, and keeping stirring at a low speed for 20-30min to obtain a dexamethasone phosphate solution; adding methylbenzene from a third feeding port, keeping stirring at a low speed for 10-20min, opening a third switch valve at the bottom of the reaction tank to enable all the solution to flow into the first standing tank, then closing the third switch valve, and starting the next preparation procedure of the reaction tank;
standing and phase splitting are carried out in a first standing tank, the oil phase is arranged at the upper part, the water phase is arranged at the lower part, a fourth switch valve is opened, the water phase is led into a first water collecting tank, the fourth switch valve is closed after the water phase is finished, a fifth switch valve is opened, and the oil phase is led into a first oil phase tank;
opening a sixth switch valve, introducing all the oil phase in the first oil phase tank into a second standing tank, opening a seventh switch valve, dropwise adding a sodium hydroxide solution into the second standing tank to enable the pH value in the second standing tank to be 10-11, standing for phase splitting, introducing the water phase into the second water collecting tank, closing an eighth switch valve, opening a ninth switch valve, and collecting the oil phase into the second oil phase tank, wherein the water phase is at the bottom and the oil phase is at the upper part, the eighth switch valve is opened, the water phase is introduced into the second water collecting tank, and after the water phase is collected, the eighth switch valve is closed, the ninth switch valve is opened;
step 4, decoloring and filtering;
opening a tenth switch valve, introducing all the aqueous phase solution into the activated carbon filter layer for decoloring and filtering, and allowing the aqueous phase solution after decoloring and filtering to flow into a collection tank; opening the eleventh switch valve, and inputting the aqueous phase solution into the multistage omentum filter through the second outlet;
and 5, crystallizing, namely fusing the water phase solution after passing through the net film filter with acetone, spraying the fused water phase solution into a crystallizing tank through a nozzle, keeping the crystallizing tank at 40-60 ℃ for 30 minutes, and then heating the upper heating block and the lower heating block to 150-180 ℃ simultaneously to perform drying crystallization.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, through multi-stage standing and phase splitting, the water phase and the oil phase are separated thoroughly, and the product precision of dexamethasone sodium phosphate is improved. In addition, the preparation conditions of firstly cooling and then heating are adopted in the reaction tank, the preparation mechanism of the dexamethasone sodium phosphate is met, and the product quality is improved. In the crystallization process, the crystal growing is formed through the heat convection of the upper heating block and the lower heating block, the crystal quality is improved, and the storage is convenient.
Drawings
The invention is illustrated and described only by way of example and not by way of limitation in the scope of the invention as set forth in the following drawings, in which:
FIG. 1: the invention has a schematic structure;
FIG. 2 is a schematic diagram: the condition control system and the reaction tank assembly are connected schematically;
FIG. 3: a structural schematic diagram of a crystallization assembly.
Detailed Description
In order to make the objects, technical solutions, design methods, and advantages of the present invention more apparent, the present invention will be further described in detail by specific embodiments with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1-3, the invention provides a preparation system of dexamethasone sodium phosphate, which comprises a condition control system, a reaction tank component and a crystallization component; the condition control system is connected with the reaction tank assembly and is used for providing low-temperature conditions and heat preservation conditions required by reaction for the reaction tank assembly; the crystallization assembly is communicated with the reaction tank body through a pipeline and is used for conveying a reaction product of the reaction tank assembly to the crystallization assembly for crystallization;
the reaction tank assembly includes: a support 55 and a can disposed on the support 55;
the jar body includes: a reaction tank, an upper cover 14 and an isolation tank body 33;
a conduction sheet is arranged outside the reaction tank, a sealed temperature control area 22 formed around the periphery of the reaction tank is arranged outside the conduction sheet, and the inner wall of the tank body is arranged outside the temperature control area 22; a first inlet 23 is formed in one side of the temperature control area 22, the first inlet 23 extends to the outside of the reaction tank, a first switch valve 24 is arranged at the first inlet 23, a first outlet 25 is formed in the other side of the temperature control area 22, the first outlet 25 extends to the outside of the reaction tank, and a second switch valve 26 is arranged at the first outlet 25;
the inside agitating unit that is provided with of retort, agitating unit include (mixing) shaft 15 and agitator motor 17, and agitator motor 17 on (mixing) shaft 15 and the 14 upper portions of upper cover pass through shaft coupling 16 and are connected.
The upper cover 14 is positioned at the top of the reaction tank, and the upper cover 14 is respectively provided with a first feed inlet 18, a second feed inlet 19, a third feed inlet 20 and a fourth feed inlet 21 which are communicated with the reaction tank;
the isolation tank body 33 is positioned at the bottom of the reaction tank, the bottom of the isolation tank body 33 is sealed and the interior of the isolation tank body 33 is hollow, the interior of the isolation tank body 33 is divided into six functional areas from top to bottom, the first functional area is a first standing tank 29, the second functional area is a first water collecting tank 44 and a first oil phase tank 38 which are arranged side by side, the third functional area is a second standing tank 39, the fourth functional area is a second oil phase tank 49 and a second water collecting tank 42 which are arranged side by side, the fifth functional area is an activated carbon filter layer 50, and the sixth functional area is a collecting tank 52;
one side of the first water collection tank 44 is connected to the water collection tank 57 through the thirteenth switching valve 36 via the third outlet 35;
a fifth feeding port is formed in the tank body shell on one side of the upper part of the second standing tank 39, a seventh switch valve 34 is arranged at the fifth feeding port, and the seventh switch valve 34 is connected with the condition control system through a pipeline;
a fourth outlet 47 is arranged on one side of the second oil phase tank 49, and the fourth outlet 47 is connected to an oil phase tank 56 through a fourteenth switching valve 48;
a second outlet 53 is arranged at the collecting tank 52, an eleventh switch valve 54 is arranged at the second outlet 53, and the second outlet 53 is connected to a multistage membrane filter 58 through the eleventh switch valve 54;
the multistage web filter 58 is in communication with the crystallization assembly.
In the above, the bottom of the reaction tank is provided with a third on-off valve 27, and the third on-off valve 27 is connected to a first standing tank 29 through a first standing input pipeline 28;
a fourth switch valve 32 and a fifth switch valve 31 are arranged at the bottom of the first standing tank 29, the fourth switch valve 32 is connected to the first water collecting tank 44 through a pipeline, and the fifth switch valve 31 is connected to the first oil phase tank 38 through a pipeline;
a sixth switching valve 41 is arranged at the bottom of the first oil phase tank 38, and the sixth switching valve 41 is connected to the second standing tank 39 through a pipeline;
an eighth switch valve 40 and a ninth switch valve 45 are arranged at the bottom of the second standing tank 39, the eighth switch valve 40 is connected to the second oil phase tank 49 through a pipeline, and the ninth switch valve 45 is connected to the second water collecting tank 42 through a pipeline;
the bottom of the second water collecting tank 42 is provided with a tenth switch valve 46, the tenth switch valve 46 is connected to the activated carbon filter layer 50, and the bottom of the activated carbon filter layer 50 is provided with a filter plate 51.
In the above, an inner lining plate is arranged on the inner wall of the insulating tank 33, a first supporting plate is arranged between the first functional region and the second functional region, and both sides of the first supporting plate are fixed on the inner lining plate;
a second support plate is arranged between the second functional area and the third functional area, and two sides of the second support plate are fixed on the inner lining plate;
a third support plate is arranged between the third functional area and the fourth functional area, and two sides of the third support plate are fixed on the inner lining plate;
a fourth supporting plate 43 is arranged between the fourth functional area and the fifth functional area, and both sides of the fourth supporting plate 43 are fixed on the inner lining plate.
As shown in fig. 2, the condition control system includes an electric cabinet 1, a control device is arranged in the electric cabinet 1, an isolation substrate 2 is arranged on the upper portion of the electric cabinet 1, a cold storage box 3 is arranged on the upper portion of the isolation substrate 2, and a base 4 is arranged on the upper portion of the cold storage box 3;
a heating fan 5 is arranged on one side of the top of the base 4; a supporting seat 6 is arranged in the middle of the top of the base 4, a refrigerating unit 9 is arranged on the upper portion of the supporting seat 6, and the refrigerating unit is connected to the cold storage box 3 through a refrigerating pipeline 8 and an electromagnetic valve 7; a sodium hydroxide solution tank is arranged on the other side of the top of the base 4;
the feeding pipeline of the sodium hydroxide solution tank is communicated with the seventh switch valve 34;
the cold accumulator 3 is communicated with the first switch valve 24 through a cold air pipe 12 and a first interface of a first two-way valve 13;
the heating fan 5 is communicated with a second interface of the first two-way valve 13 through a hot air pipeline 10;
the cold accumulator 3 is communicated with the second switch valve 26 through the return pipeline 11 and a first interface of the second two-way valve 13, and a second interface of the second two-way valve 13 leads to the outside of the reaction tank.
As shown in fig. 3, the crystallization assembly includes a crystallization tank 78 and an acetone storage tank 81;
a recovery port 67 is formed in one side of the top of the crystallizing tank 78, a nozzle 65 is arranged in the center of the top of the crystallizing tank 78, a pressurizing device 63 is arranged at the top of the nozzle 65, and a pressurizing pipe 64 is arranged on one side of the pressurizing device 63; the bottom of the crystallizing tank 78 is provided with a discharge port 77, and the discharge port 77 is connected to a crystal collecting tank 80 through a pipeline and a fifteenth switch valve 76;
the multistage mesh membrane filter 58 is communicated with a first port of a three-way valve through an aqueous solution pipeline 59, the acetone storage tank 81 is communicated with a second port of the three-way valve through a pipeline and a sixteenth switch valve 82, and a third port of the three-way valve is communicated with the pressurizing device 63 through a mixer 61 and a twelfth switch valve 62;
In the above, the top of the recovery port 67 is provided with an exhaust valve assembly;
the exhaust valve assembly comprises a valve body 72 and a stroke seat 70, one end of the valve body 72 is butted with the recovery port 67, and the stroke seat 70 is arranged at the upper part of the valve body 72;
a film pressure plate 71 is arranged inside the valve body 72, a film 74 transversely penetrating through the film pressure plate 71 is embedded in the film pressure plate 71, and two sides of the film 74 are fixed on fixing lugs inside the valve body 72;
a shaft rod 69 is arranged at the upper part of the film pressure plate 71, a spring 68 is arranged outside the shaft rod 69, the spring 68 is clamped at the joint of the stroke seat 70 and the valve body 72, a sealing seat is arranged between the stroke seat 70 and the valve body 72, and the shaft rod 69 penetrates through the sealing seat. A temperature controller 79 is arranged on one side of the crystallizing tank 78, and the temperature controller 79 is used for controlling the temperature of the heating wire.
For better implementation, the first to sixteenth switching valves 24 to 82 are respectively connected with a control device in the electric cabinet 1; the first feeding port 18, the second feeding port 19, the third feeding port 20, the fourth feeding port 21 and the fifth feeding port are respectively provided with a metering pump.
The second aspect of the invention provides a preparation process of dexamethasone sodium phosphate, which comprises the following steps:
1: preparation of dexamethasone phosphate solution
Adding 200L of anhydrous tetrahydrofuran into a reaction tank through a first feeding port 18, adding 100mol of dexamethasone into the reaction tank through a second feeding port 19, controlling a motor 17 to start, and driving a stirring shaft 15 to stir at a low speed for 25 minutes by the motor through a coupler 16 so as to ensure that the mixture is fully dispersed; controlling the first two-way valve 13 to be opened, enabling cold air at-70 ℃ in the cold accumulator 3 to flow through the cold air pipe 12, the first two-way valve 13, the first switch valve 24 and the first inlet 23 to enter the temperature control area 22, refrigerating low-temperature gas in the temperature control area 22 through a guide sheet, enabling the temperature inside the reaction tank to be reduced to-55 ℃, keeping the low-temperature environment at-55 ℃ unchanged, adding 300mol of pyrophosphate into the reaction tank, continuing to stir at a low speed for 80min, adding 100L of pure water for hydrolysis, opening the second switch valve 26 and the second two-way valve 37 at the first outlet 25 in the hydrolysis process, injecting the cold air into the cold accumulator through the return pipeline 11, closing an electromagnetic valve on the return pipeline 11 when 70% of the cold air is discharged, controlling the first two-way valve to be connected with the hot air pipeline, enabling the heating fan 5 to enable hot air to flow through the hot air pipeline 10, the first two-way valve 24, the first inlet 23 and the temperature control area 22, keeping the second switch valve 26 at the first outlet 25 open, enabling the hot air pipeline to flow to be heated and gradually heated and stirring the temperature of the phosphoric acid ester to be heated and gradually increased to obtain a temperature reaction solution, and the dexamethasone solution, wherein the dexamethasone is discharged.
Then 150L of toluene is added from the third feeding port 20, the stirring is kept at a low speed for 15min, then the third switch valve 27 at the bottom of the reaction tank is opened to allow the solution to flow into the first standing tank 29 completely, then the third switch valve 27 is closed, the reaction tank starts the next preparation process,
2: standing for the first time to split the phase, and collecting an oil phase;
standing in a first standing tank 29 for 2H to perform phase separation, wherein the oil phase is at the upper part and the water phase is at the lower part, then opening a fourth switch valve 32, introducing the water phase into a first water collecting tank 44, closing the fourth switch valve 32 after the water phase is finished, opening a fifth switch valve 31, and introducing the oil phase into a first oil phase tank 38;
3: carrying out secondary standing and phase splitting, and collecting a water phase;
opening a sixth switch valve 41 at the bottom of the first oil phase tank 38, introducing all the oil phases in the first oil phase tank into a regulating tank 39, opening a seventh switch valve 34 at the upper part of the regulating tank 39, dropwise adding a sodium hydroxide solution into the regulating tank to adjust the pH of the interior of the regulating tank to 10.5, standing for 1h in the regulating tank for phase splitting, opening an eighth switch valve 40 at the bottom of the regulating tank with the water phase at the bottom and the oil phase at the upper part, introducing the water phase into a second water collecting tank 42, after the water phase is collected, closing the eighth switch valve 40, opening a ninth switch valve 45, and collecting the oil phase into a second oil phase tank 49;
4: the color is removed and filtered, and then the mixture is filtered,
opening a tenth switch valve 46 at the bottom of the second water collecting tank 42, introducing all the aqueous phase solution into an activated carbon filter layer 50 for decolorization and filtration, and allowing the aqueous phase solution after decolorization and filtration to flow into a collecting tank 52; opening the eleventh on-off valve 54 at the collection tank 52 to feed the aqueous phase solution to the multistage omentum filter, 58, through the second outlet;
5: crystallizing, after the aqueous phase solution and the acetone which pass through the membrane filter 58 are fused, the aqueous phase solution and the acetone pass through a mixer 61 and a twelfth switch valve 62 and then reach a pressurizing device 63, wherein a pressurizing pipe 64 is arranged on one side of the pressurizing device 63, after the aqueous phase solution and the acetone are fused, the mixed solution of the aqueous phase solution and the acetone is sprayed into a crystallizing tank 78 through a nozzle 65 by high-pressure gas at the pressurizing device 63, so that the aqueous phase solution and the acetone are fully dispersed and fused, simultaneously, an upper heating wire and a lower heating wire on the upper portion and the lower portion of the crystallizing tank are opened to respectively heat an upper heating block and a lower heating block, so that the upper heating block and the lower heating block are simultaneously heated to 50 ℃, thermal convection of the upper heating block and the lower heating block forms crystal growth, crystal growth is kept for 30 minutes, and then the upper heating block and the lower heating block are simultaneously heated to 165 ℃ for drying and crystallizing.
While embodiments of the present invention have been described above, the above description is illustrative, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or improvements made to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (9)
1. A preparation system of dexamethasone sodium phosphate is characterized by comprising a condition control system, a reaction tank component and a crystallization component;
the condition control system is connected with the reaction tank assembly and at least used for providing low-temperature conditions and heat preservation conditions required by reaction for the reaction tank assembly;
the crystallization assembly is communicated with the reaction tank body through a pipeline and is used for conveying a reaction product of the reaction tank assembly to the crystallization assembly for crystallization;
the reaction tank assembly includes: the tank comprises a support (55) and a tank body arranged on the support (55);
the jar body includes: the reaction tank, the upper cover (14) and the isolation tank body (33);
a conduction sheet is arranged outside the reaction tank, a sealed temperature control area (22) formed around the periphery of the reaction tank is arranged outside the conduction sheet, and the inner wall of the tank body is arranged outside the temperature control area (22); a first inlet (23) is formed in one side of the temperature control area (22), the first inlet (23) extends to the outside of the reaction tank, a first switch valve (24) is arranged at the first inlet (23), a first outlet (25) is formed in the other side of the temperature control area (22), the first outlet (25) extends to the outside of the reaction tank, and a second switch valve (26) is arranged at the first outlet (25);
a stirring device is arranged in the reaction tank;
the upper cover (14) is positioned at the top of the reaction tank, and a first feed inlet (18), a second feed inlet (19), a third feed inlet (20) and a fourth feed inlet (21) which are communicated with the reaction tank are respectively arranged on the upper cover (14);
the isolation tank body (33) is located at the bottom of the reaction tank, the bottom of the isolation tank body (33) is sealed and hollow, the interior of the isolation tank body (33) is divided into six functional areas from top to bottom, the first functional area is a first standing tank (29), the second functional area is a first water collecting tank (44) and a first oil phase tank (38) which are arranged side by side, the third functional area is a second standing tank (39), the fourth functional area is a second oil phase tank (49) and a second water collecting tank (42) which are arranged side by side, the fifth functional area is an activated carbon filter layer (50), and the sixth functional area is a collection tank (52);
one side of the first water collection tank (44) is connected to a water collection tank (57) through a thirteenth switching valve (36) through a third outlet (35);
a fifth feeding port is formed in the shell of the tank body on one side of the upper part of the second standing tank (39), a seventh switch valve (34) is arranged at the fifth feeding port, and the seventh switch valve (34) is connected with the condition control system through a pipeline;
a fourth outlet (47) is formed in one side of the second oil phase tank (49), and the fourth outlet (47) is connected to an oil phase tank (56) through a fourteenth switching valve (48);
a second outlet (53) is arranged at the collecting tank (52), an eleventh switch valve (54) is arranged at the second outlet (53), and the second outlet (53) is connected to the multistage mesh membrane filter (58) through the eleventh switch valve (54);
the multistage web filter (58) is in communication with the crystallization assembly.
2. The preparation system of dexamethasone sodium phosphate according to claim 1, wherein a third on-off valve (27) is arranged at the bottom of the reaction tank, and the third on-off valve (27) is connected to a first still tank (29) through a first still input pipeline (28);
a fourth switch valve (32) and a fifth switch valve (31) are arranged at the bottom of the first standing tank (29), the fourth switch valve (32) is connected to the first water collecting tank (44) through a pipeline, and the fifth switch valve (31) is connected to the first oil phase tank (38) through a pipeline;
a sixth switching valve (41) is arranged at the bottom of the first oil phase tank (38), and the sixth switching valve (41) is connected to the second standing tank (39) through a pipeline;
an eighth switch valve (40) and a ninth switch valve (45) are arranged at the bottom of the second standing tank (39), the eighth switch valve (40) is connected to the second oil phase tank (49) through a pipeline, and the ninth switch valve (45) is connected to the second water collecting tank (42) through a pipeline;
the bottom of the second water collecting tank (42) is provided with a tenth switch valve (46), the tenth switch valve (46) is connected to the activated carbon filter layer (50), and the bottom of the activated carbon filter layer (50) is provided with a filter plate (51).
3. The preparation system of dexamethasone sodium phosphate as claimed in claim 1, wherein an inner lining plate is arranged on the inner wall of the isolation tank (33), a first support plate is arranged between the first functional region and the second functional region, and two sides of the first support plate are fixed on the inner lining plate;
a second support plate is arranged between the second functional area and the third functional area, and two sides of the second support plate are fixed on the inner lining plate;
a third support plate is arranged between the third functional area and the fourth functional area, and two sides of the third support plate are fixed on the inner lining plate;
a fourth supporting plate (43) is arranged between the fourth functional area and the fifth functional area, and two sides of the fourth supporting plate (43) are fixed on the inner lining plate.
4. The preparation system of dexamethasone sodium phosphate as claimed in claim 1, wherein the condition control system comprises an electric cabinet (1), an isolation substrate (2) is arranged on the upper part of the electric cabinet (1), a cold storage tank (3) is arranged on the upper part of the isolation substrate (2), and a base (4) is arranged on the upper part of the cold storage tank (3);
a heating fan (5) is arranged on one side of the top of the base (4); a supporting seat (6) is arranged in the middle of the top of the base (4), a refrigerating unit (9) is arranged on the upper portion of the supporting seat (6), and the refrigerating unit is connected to the cold storage box (3) through a refrigerating pipeline (8) and an electromagnetic valve (7); a sodium hydroxide solution tank is arranged on the other side of the top of the base (4);
the feeding pipeline of the sodium hydroxide solution tank is communicated with the seventh switch valve (34);
the cold accumulator (3) is communicated with the first switch valve (24) through a cold air pipe (12) and a first interface of a first two-way valve (13);
the heating fan (5) is communicated with a second interface of the first two-way valve (13) through a hot air pipeline (10);
the cold accumulator (3) is communicated with the second switch valve (26) through a return pipeline (11) and a first interface of the second two-way valve (13), and a second interface of the second two-way valve (13) is communicated with the outside of the reaction tank.
5. The system for preparing dexamethasone sodium phosphate according to claim 1, wherein the crystallization component comprises a crystallization tank (78) and an acetone storage tank (81);
a recovery opening (67) is formed in one side of the top of the crystallizing tank (78), a nozzle (65) is arranged in the center of the top of the crystallizing tank (78), a pressurizing device (63) is arranged at the top of the nozzle (65), and a pressurizing pipe (64) is arranged on one side of the pressurizing device (63); a discharge port (77) is formed in the bottom of the crystallization tank (78), and the discharge port (77) is connected to a crystal collecting tank (80) through a pipeline and a fifteenth switch valve (76);
the multistage mesh membrane filter (58) is communicated with a first port of a three-way valve through a water phase solution pipeline (59), the acetone storage tank (81) is communicated with a second port of the three-way valve through a pipeline and a sixteenth switch valve (82), and a third port of the three-way valve is communicated with the pressurizing device (63) through a mixer (61) and a twelfth switch valve (62);
crystallizer (78) top is provided with heating block (67), and the crystallizer bottom is provided with down heating block (75), it all is provided with the heater strip with heating block (75) inside down to go up heating block (67).
6. The dexamethasone sodium phosphate preparation system according to claim 5, wherein a gas discharge valve assembly is arranged at the top of the recovery port (67);
the exhaust valve assembly comprises a valve body (72) and a stroke seat (70), one end of the valve body (72) is butted with the recovery port (67), and the stroke seat (70) is arranged at the upper part of the valve body (72);
a film pressure plate (71) is arranged in the valve body (72), a film (74) transversely penetrating through the film pressure plate (71) is embedded in the film pressure plate (71), and two sides of the film (74) are fixed on fixing lugs in the valve body (72);
the upper part of the film pressure plate (71) is provided with a shaft rod (69), a spring (68) is arranged outside the shaft rod (69), the spring (68) is clamped at the joint of the stroke seat (70) and the valve body (72), a sealing seat is arranged between the stroke seat (70) and the valve body (72), and the shaft rod (69) penetrates through the sealing seat.
7. The dexamethasone sodium phosphate preparation system according to claim 6, wherein a temperature controller (79) is arranged on one side of the crystallization tank (78), and the temperature controller (79) is used for controlling the temperature of the heating wire.
8. The preparation system of dexamethasone sodium phosphate according to any one of claims 1 to 7, wherein the first through sixteenth switching valves (24) through (82) are respectively connected with a control device in the electric cabinet (1);
and metering pumps are respectively arranged at the first feeding port (18), the second feeding port (19), the third feeding port (20), the fourth feeding port (21) and the fifth feeding port.
9. A preparation process of dexamethasone sodium phosphate, which is characterized in that the preparation process applies the preparation system of claim 8, and comprises the following steps:
step 1, preparing a dexamethasone phosphate solution:
anhydrous tetrahydrofuran is added into a reaction tank from a first feeding port (18), dexamethasone is added into the reaction tank from a second feeding port (19) to be stirred, a first two-way valve (13) is controlled to be opened, so that cold airflow at-70 ℃ in a cold accumulator (3) enters a temperature control area (22), the temperature inside the reaction tank is reduced to-55 ℃, pyrophosphoryl chloride is added into the reaction tank, and stirring is carried out; adding pure water for hydrolysis, discharging cold air in the reaction tank, closing an electromagnetic valve on a return pipeline (11) when the cold air is discharged by more than 70%, feeding hot air into a temperature control area (22) by a heating fan (5), and simultaneously keeping a second switch valve (26) open, so that the temperature of the reaction tank is gradually increased to 25-30 ℃, and stirring at a low speed for 20-30min to obtain a dexamethasone phosphate solution; adding toluene from a third feeding port (20), keeping stirring at a low speed for 10-20min, opening a third switch valve (27) at the bottom of the reaction tank to enable the solution to completely flow into a first standing tank (29), then closing the third switch valve (27), and starting the next preparation process of the reaction tank;
step 2, standing for phase splitting once, and collecting an oil phase;
standing and phase splitting are carried out in a first standing tank (29), the oil phase is arranged at the upper part, the water phase is arranged at the lower part, a fourth switch valve (32) is opened, the water phase is led into a first water collecting tank (44), the fourth switch valve (32) is closed after the water phase is finished, a fifth switch valve (31) is opened, and the oil phase is led into a first oil phase tank (38);
step 3, standing for the second time for phase splitting, and collecting a water phase;
opening a sixth switch valve (41), introducing all the oil phase in the first oil phase tank (38) into a second standing tank (39), opening a seventh switch valve (34), dropwise adding a sodium hydroxide solution into the second standing tank (39) to enable the pH value in the second standing tank (39) to be 10-11, standing for phase separation, opening an eighth switch valve (40) when the water phase is at the bottom and the oil phase is at the upper part, introducing the water phase into a second water collecting tank (42), closing the eighth switch valve (40), opening a ninth switch valve (45) after the water phase is collected, and collecting the oil phase into a second oil phase tank (49);
step 4, decoloring and filtering;
opening a tenth switch valve (46), introducing all the aqueous phase solution into an activated carbon filter layer (50) for decolorization and filtration, and allowing the aqueous phase solution after decolorization and filtration to flow into a collection tank (52); opening the eleventh on-off valve 54 to feed the aqueous phase solution to the multistage mesh membrane filter (58) through the second outlet;
and step 5, crystallizing, namely fusing the water-phase solution passing through the membrane filter 58 with acetone, spraying the fused solution into a crystallizing tank (78) through a nozzle (65), keeping the crystallizing tank (78) at 40-60 ℃ for crystallizing for 30 minutes, and then simultaneously heating the upper heating block and the lower heating block to 150-180 ℃ for drying and crystallizing.
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