CN108912193B - Production process and production device of medroxyprogesterone acetate - Google Patents
Production process and production device of medroxyprogesterone acetate Download PDFInfo
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- CN108912193B CN108912193B CN201810826736.2A CN201810826736A CN108912193B CN 108912193 B CN108912193 B CN 108912193B CN 201810826736 A CN201810826736 A CN 201810826736A CN 108912193 B CN108912193 B CN 108912193B
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- 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
- C07J7/004—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 substituted in position 17 alfa
- C07J7/0045—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 substituted in position 17 alfa not substituted in position 16
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B11/00—Machines or apparatus for drying solid materials or objects with movement which is non-progressive
- F26B11/02—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles
- F26B11/08—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles rotating about a vertical or steeply-inclined axis
- F26B11/10—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles rotating about a vertical or steeply-inclined axis with stirring devices which are held stationary
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/001—Drying-air generating units, e.g. movable, independent of drying enclosure
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/04—Agitating, stirring, or scraping devices
Abstract
The invention discloses a medroxyprogesterone acetate production device, which comprises a reaction kettle, a elutriation kettle, a centrifugal machine, a concentration kettle, a decoloring kettle and drying equipment, wherein the drying equipment comprises an outer cylinder, a drying cylinder and an inner cylinder; the bottom surface of the outer barrel is provided with a motor, and an exhaust fan blade, a barrel type impeller and a vortex impeller are arranged on a rotating shaft of the motor; the exhaust fan blades are arranged between the drying cylinder and the bottom surface of the outer cylinder; the drum type impeller is arranged between the drying drum and the inner drum; the vortex impeller is arranged at the bottom of the inner cylinder; the top surface of the inner cylinder is provided with an infrared heating pipe; the upper end of the interlayer cavity of the outer barrel is provided with an air purification ring; a feed inlet is arranged in the center of the top plate, and a support is arranged above the feed inlet; two sides in the bracket are provided with screw rods connected with a driving motor; the screw rod is provided with a cover plate; the lower end of the cover plate is provided with a suspender, and positioning blocks for supporting the supporting plate are uniformly arranged on the suspender; the supporting plate is horizontally arranged between the hanging rods. The invention can reduce the preparation time of the intermediate product in the production process of medroxyprogesterone acetate and realize the rapid high-quality production of medroxyprogesterone acetate.
Description
Technical Field
The invention belongs to the technical field of medicine production, and particularly relates to a medroxyprogesterone acetate production process and a production device.
Background
the traditional medroxyprogesterone acetate is produced by adopting multi-step chemical reactions, and the formed intermediate product raw materials need to be dried for multiple times, while the existing drying equipment generally adopts electrothermal filament heating drying or complete vacuum pumping negative pressure dehumidification, the electrothermal filament heating drying easily generates larger negative influence on the intermediate product for preparing the medroxyprogesterone acetate, so that the structure of the intermediate product is changed, and the subsequent crystallization of the medroxyprogesterone acetate is unstable, the purity is reduced, and meanwhile, the drying time is longer regardless of the existing electrothermal filament heating drying equipment or vacuum pumping negative pressure dehumidification equipment, and the vacuum pumping negative pressure dehumidification can realize quick dehumidification by adopting a quick pressure reduction mode, but the quick shape and the structure of the intermediate product are easy to be damaged, and the quality of the medroxyprogesterone acetate is reduced.
Disclosure of Invention
The invention aims to solve the problems, and provides a medroxyprogesterone acetate production device, which adopts flexible drying equipment for adjustment, can form a gentle local vortex type heat negative pressure effect, does not damage the material structure, can quickly dry, reduces the preparation time of an intermediate product in the medroxyprogesterone acetate production process, and realizes the quick high-quality production of medroxyprogesterone acetate.
In order to realize the purpose, the invention adopts the technical scheme that: a medroxyprogesterone acetate production device comprises a reaction kettle, a elutriation kettle, a centrifuge, a concentration kettle, a decoloration kettle and a drying device which are connected with each other according to working procedures, wherein the drying device comprises an outer cylinder, a drying cylinder is coaxially arranged in the outer cylinder, and an inner cylinder is coaxially arranged in the drying cylinder; the upper ends of the outer cylinder, the drying cylinder and the inner cylinder are all connected with a top plate; a motor is arranged in the center of the bottom surface of the outer cylinder, and a rotating shaft at the top end of the motor extends into the inner cylinder; the exhaust fan blades, the cylindrical impeller and the vortex impeller are sequentially arranged on the rotating shaft from bottom to top; the exhaust fan blades are arranged between the bottom surface of the drying cylinder and the bottom surface of the outer cylinder; the drum type impeller is arranged between the drying drum and the inner drum; the vortex impeller is arranged at the bottom of the inner cylinder; the top surface of the inner cylinder is provided with an annular infrared heating pipe; the side wall of the drying cylinder is a double-layer mesh plate, and a drying agent is filled in an interlayer of the double-layer mesh plate; the side wall of the inner cylinder is a mesh plate; the side wall of the outer barrel comprises an inner layer wall and an outer layer wall; an interlayer cavity is formed between the inner layer wall and the outer layer wall; the lower end of the inner wall is provided with an exhaust hole communicated with the interlayer cavity; an annular baffle is arranged at an outlet at the upper end of the interlayer cavity; vent holes are uniformly arranged on the baffle in an annular shape; the upper end of the baffle is provided with a rotatable air purification ring; an air filter used for shielding the air vent is arranged on the air purification ring; a feed inlet is formed in the center of the top plate, and an inverted U-shaped support is arranged above the feed inlet; screw rods connected with a driving motor are arranged on two sides in the bracket; the screw rod is provided with a cover plate capable of lifting up and down; a hanging rod is vertically arranged at the lower end of the cover plate, and positioning blocks for supporting the supporting plate are uniformly arranged on the hanging rod; the supporting plate is horizontally arranged between the hanging rods.
Further, the driving motor is arranged at the top end of the bracket; a pinion is arranged at the upper end of the screw rod; the pinion is connected with a driving gear on the driving motor through a chain.
Furthermore, four hanging rods are arranged at the lower end of the cover plate and are distributed in a rectangular shape; the bottom end of the suspender is connected with the fixing frame.
Furthermore, infrared heating lamps are distributed on the inner wall of the inner-layer wall.
Furthermore, ultraviolet lamps are distributed in the interlayer cavity.
Furthermore, a pressure gauge is arranged on the cover plate.
Further, the vortex impeller comprises a blade rod arranged on the rotating shaft, and a vertical blade is arranged at the end of the blade rod; the vertical blades comprise vertical plates perpendicular to the horizontal plane, and inclined plates inclined to the horizontal plane are integrally arranged at the upper ends of the vertical plates.
Furthermore, the bottom surface of the inner cylinder is provided with two layers, including a lower bottom plate at the lower layer and a disc plate at the upper layer; connecting rods are uniformly arranged at the edge of the disc plate and connected with the inner wall of the inner cylinder; the vortex impeller is arranged between the lower bottom plate and the disc plate; the disc plate shields the blade rods.
Further, the barrel impeller includes an upper mounting ring and a lower mounting ring; straight blades are uniformly distributed between the upper mounting ring and the lower mounting ring in an annular manner; the lower mounting ring is coaxially connected with the rotating shaft through a mounting rod; the upper mounting ring is arranged on the bottom surface of the top plate through a bearing.
Furthermore, the reflecting cover of the infrared heating pipe is conical.
Another objective of the present invention is to provide a process for producing medroxyprogesterone acetate, which can shorten the production time of medroxyprogesterone acetate by using the above-mentioned production apparatus, comprising the following steps:
preparation of acetic acid methine:
pumping 400-500 parts of tetrahydrofuran into a reaction kettle, adding 130-170 parts of 17 α -hydroxyprogesterone acetate, stirring, pumping 50-70 parts of triethyl orthoformate and 70-90 parts of absolute ethyl alcohol, introducing nitrogen, adding 2-4 parts of PTS, carrying out heat preservation reaction at 34-36 ℃ for 0.8-1.5 hours, adding 2-4 parts of PTS, reacting for 1-2 hours, cooling to 25-30 ℃, sequentially pumping 40-50 parts of N-methylaniline and 40-50 parts of formaldehyde, heating to 34-36 ℃ for reaction for 2-3 hours, pumping a reaction liquid into a elutriation kettle, cooling to 10-20 ℃, dropwise adding 150-200 parts of hydrochloric acid, carrying out heat preservation reaction at 23-27 ℃ for 1-2 hours, slowly adding 1400-1600 parts of water for elutriation, cooling to 4-6 ℃, stirring for 2-4 hours, centrifuging, washing to be neutral, putting into a drying device, starting an infrared heating pipe 6, irradiating for 8-12 minutes, controlling the rotation speed of a motor 19 to be 1000-1300r/min, continuously operating for 10-15 minutes, and obtaining acetic acid methyl acetate;
the reaction formula is as follows:
hydrogenation reaction:
pumping 400-500 parts of DMF (dimethyl formamide) into a reaction kettle, adding 130-170 parts of the acetic acid methine, introducing nitrogen, adding 20-30 parts of palladium carbon and 50-70 parts of cyclohexene, heating to 96-100 ℃ for reaction for 2-3 hours, filtering to a transposition kettle, cooling the filtrate to 15-25 ℃, adding 15-20 parts of hydrochloric acid, keeping the temperature for 1-2 hours at 20-22 ℃ after the addition is finished, adding 15-20 parts of sodium bicarbonate, cooling to 0 ℃ after the addition is finished, keeping the temperature for 2-4 hours, centrifuging, washing with water, spin-drying, and drying to obtain a crude product; adding 500-600 parts of dichloromethane, 800-820 parts of ethanol, 120-140 parts of the crude product and 12-14 parts of activated carbon into a decoloring kettle, heating to 35-45 ℃ for reflux, decoloring for 20-40 minutes, concentrating the filtrate in a filter paper concentrating kettle to a small volume of about 2V mother liquor, cooling to 0-5 ℃ for crystallization for 1.5-2.5 hours, centrifuging and drying, putting the product into a drying device, starting an infrared heating pipe 6, irradiating for 8-12 minutes, controlling the rotating speed of a motor 19 to be 1300-1500r/min, and continuously operating for 10-15 minutes to obtain a refined medroxyprogesterone acetate product;
the reaction formula is as follows:
preferably, the process for producing medroxyprogesterone acetate comprises the following preparation steps:
preparation of acetic acid methine:
pumping 450 parts of tetrahydrofuran into a reaction kettle, adding 150 parts of 17 α -hydroxyprogesterone acetate, stirring, pumping 60 parts of triethyl orthoformate and 80 parts of absolute ethyl alcohol, introducing nitrogen, adding 3 parts of PTS, carrying out heat preservation reaction at 34-36 ℃ for 1 hour, adding 3 parts of PTS, carrying out reaction for 1.5 hours, reducing the temperature to 28 ℃, sequentially pumping 45 parts of N-methylaniline and 45 parts of formaldehyde, heating to 34-36 ℃ for 2.5 hours, pumping the reaction liquid into a elutriation kettle, reducing the temperature to 15 ℃, dropwise adding 180 parts of hydrochloric acid, completing dropwise addition within 30 minutes, carrying out heat preservation reaction at 23-27 ℃ for 1.5 hours, slowly adding 1500 parts of elutriation, reducing the temperature to 5 ℃, stirring for 3 hours, centrifuging, washing to be neutral, putting into the drying equipment, starting an infrared heating pipe 6, irradiating for 8-12 minutes, controlling the rotation speed of a motor 19 to be 1000-1300r/min, and continuously operating for 10-15 minutes to obtain acetic acid methine;
hydrogenation reaction:
pumping 450 parts of DMF into a reaction kettle, adding 150 parts of the acetic acid methine, introducing nitrogen, adding 24 parts of palladium-carbon and 60 parts of cyclohexene, heating to 96-100 ℃, reacting for 2 hours and 40 minutes, filtering to a transposition kettle, cooling the filtrate to 20 ℃, adding 18 parts of hydrochloric acid, preserving heat for 1.5 hours at 20-22 ℃, adding 18 parts of sodium bicarbonate, cooling to 0 ℃ after adding, preserving heat for 3 hours, centrifuging, washing with water, spin-drying, and drying to obtain a crude product; adding 540 parts of dichloromethane, 810 parts of ethanol, 135 parts of the crude product and 13.5 parts of activated carbon into a decoloring kettle, heating to 40 ℃ for reflux, decoloring for 30 minutes, filtering a paper concentrating kettle, concentrating to a small volume, cooling to 0-5 ℃ for crystallization for 2 hours, centrifuging, spin-drying, putting into a drying device, starting an infrared heating pipe 6, irradiating for 8-12 minutes, controlling the rotating speed of a motor 19 to be 1300-1500r/min, and continuously operating for 10-15 minutes to obtain the refined medroxyprogesterone acetate.
The invention has the beneficial effects that:
1. compared with the traditional drying equipment, after the production device is adopted, the whole production time of the medroxyprogesterone acetate is shortened by about 30 percent, and the finished product ratio is improved by 20 to 30 percent.
2. The height position of the supporting plate in the drying equipment can be adjusted, the placement of materials is not influenced, a user can adjust the upper position and the lower position of the supporting plate in the inner cylinder, the more the supporting plate is, the stronger the heating effect of the infrared heating pipe is, the faster the negative pressure forming speed is, the more the supporting plate is, the weaker the heating effect of the infrared heating pipe is, and the slower the negative pressure forming speed is, so that the use flexibility of the drying equipment is greatly improved.
3. The drying equipment provided by the invention adopts a vortex type negative pressure illumination drying equipment which is provided with a plurality of groups of coaxial impellers to rotate and is matched with the cylinders with the multi-layer inner wall to form low negative pressure at the local part, high negative pressure at the middle part and normal external air pressure, and combines the advantages of negative pressure drying and heating drying, so that the drying speed is increased, the influence on the material is reduced, and the drying quality is ensured.
4. The inner part of the inner cylinder does not form negative pressure integrally, but the middle part forms a local negative pressure effect, and the negative pressure can disappear greatly immediately after the motor stops, so that the influence on the form of the material is very small, the form and the structure of an intermediate product are ensured, and the subsequent production quality of the medroxyprogesterone acetate is ensured.
5. According to the invention, after the material is dried, the motor can be controlled to rotate reversely, so that external air reversely enters the inner cylinder of the equipment, the internal air pressure is quickly recovered to be normal, the material is prevented from being changed in form, the equipment is convenient for a user to start, and the cooling speed of the material can be increased when external cold air enters the equipment in the reverse rotation process of the motor.
Drawings
FIG. 1 is a flow chart of the process for preparing medroxyprogesterone acetate according to the invention.
Fig. 2 is a schematic view of the internal overall structure of the vortex type negative pressure illumination drying device of the present invention.
Fig. 3 is a schematic structural view of the vortex type negative pressure illumination drying device without the drying cylinder.
Fig. 4 is a schematic sectional structure view of the drying cylinder.
Fig. 5 is an enlarged structural diagram of a part a in fig. 2.
Fig. 6 is a schematic sectional structure view of the vortex type negative pressure illumination drying apparatus.
Fig. 7 is a schematic sectional view of an overall 3D structure of an impeller device in the vortex type negative pressure illumination drying apparatus.
Fig. 8 is a schematic top view of the vortex impeller.
FIG. 9 is a schematic side view of a vertical blade on a vortex impeller.
Fig. 10 is a schematic top view of the vortex type negative pressure illumination drying device without the air purification ring.
Fig. 11 is a schematic top view of the air cleaning ring.
FIG. 12 is a schematic top view of the disk plate;
FIG. 13 is a bottom view of the discharge device;
fig. 14 is a schematic view of the connection structure between the driving motor and the chain and pinion on the bracket.
In the figure: 1. an outer cylinder; 2. a drying cylinder; 3. an inner barrel; 4. a material discharger; 5. a cover plate; 6. an infrared heating pipe; 7. a top plate; 8. a vortex impeller; 9. a barrel-type impeller; 10. an exhaust fan blade; 11. an inner wall; 12. an outer wall; 13. an upper bottom surface; 14. a ventilation hole; 15. a lower bottom surface; 16. an infrared heating lamp; 17. an interlayer cavity; 18. an ultraviolet lamp; 19. a motor; 20. a rotating shaft; 21. an outer wall; 22. a desiccant; 23. an inner wall; 24. the bottom surface of the drying cylinder; 26. an air exhaust hole; 31. an inner cylinder wall; 32. a disc plate; 33. a connecting rod; 34. a lower base plate; 41. a support plate; 42. a fixing frame; 43. a boom; 44. positioning blocks; 45. a support; 46. a drive motor; 47. a chain; 48. a pinion gear; 49. a screw rod; 50. a feed inlet; 51. a pressure gauge; 52. a handle; 71. a baffle plate; 72. a vent; 74. an air purification ring; 73. an air filter; 75. a vent channel; 81. a blade bar; 82. erecting the blades; 821. a vertical plate; 822. a sloping plate; 91. a straight blade; 92. an upper mounting ring; 93. a lower mounting ring; 94. and (5) installing a rod.
Detailed Description
The following detailed description of the present invention is given for the purpose of better understanding technical solutions of the present invention by those skilled in the art, and the present description is only exemplary and explanatory and should not be construed as limiting the scope of the present invention in any way.
As shown in fig. 1 to 14, the specific structure of the present invention is: the device comprises a reaction kettle, a elutriation kettle, a centrifuge, a concentration kettle, a decoloration kettle and drying equipment which are connected with one another according to the working procedures, wherein the drying equipment comprises an outer cylinder 1, a drying cylinder 2 is coaxially arranged in the outer cylinder 1, and an inner cylinder 3 is coaxially arranged in the drying cylinder 2; the upper ends of the outer cylinder 1, the drying cylinder 2 and the inner cylinder 3 are all connected with a top plate 7; a motor 19 is arranged in the center of the bottom surface of the outer cylinder 1, and a rotating shaft 20 at the top end of the motor 19 extends into the inner cylinder 3; the exhaust fan blades 10, the cylindrical impeller 9 and the vortex impeller 8 are sequentially arranged on the rotating shaft 20 from bottom to top; the exhaust fan blades 10 are arranged between the bottom surface 24 of the drying cylinder and the bottom surface of the outer cylinder 1; the drum type impeller 9 is arranged between the drying drum 2 and the inner drum 3; the vortex impeller 8 is arranged at the bottom of the inner barrel 3; the top surface of the inner cylinder 3 is provided with an annular infrared heating pipe 6; the side wall of the drying cylinder 2 is a double-layer mesh plate, and a drying agent 22 is filled in an interlayer of the double-layer mesh plate; the side wall of the inner cylinder 3 is a mesh plate; the side wall of the outer cylinder 1 comprises an inner layer wall 11 and an outer layer wall 12; an interlayer cavity 17 is formed between the inner layer wall 11 and the outer layer wall 12; the lower end of the inner wall 11 is provided with an exhaust hole 26 communicated with the interlayer cavity 17; an annular baffle 71 is arranged at an outlet at the upper end of the interlayer cavity 17; vent holes 72 are uniformly arranged on the baffle 71 in a ring shape; the upper end of the baffle 71 is provided with a rotatable air purification ring 74; an air filter 73 for shielding the air vent 72 is arranged on the air purification ring 74; a feed inlet 50 is formed in the center of the top plate 7, and an inverted U-shaped bracket 45 is arranged above the feed inlet 50; screw rods 49 connected with a driving motor 46 are arranged on two sides in the bracket 45; the screw rod 49 is provided with a cover plate 5 which can be lifted up and down; a hanging rod 43 is vertically arranged at the lower end of the cover plate 5, and positioning blocks 44 for supporting the supporting plate 41 are uniformly arranged on the hanging rod 43; the pallet 41 is horizontally disposed between the hanger rods 43.
Preferably, the driving motor 46 is arranged at the top end of the bracket 45; a pinion 48 is arranged at the upper end of the screw rod 49; the pinion gear 48 is connected to a drive gear on the drive motor 46 by a chain 47.
Preferably, the lower end of the cover plate 5 is provided with four suspension rods 43 which are distributed in a rectangular shape; the bottom end of the hanger bar 43 is connected with the fixed frame 42.
In order to increase the moisture discharge rate, infrared heating lamps 16 are distributed on the inner wall of the inner wall 11.
In order to realize the sterilization effect, ultraviolet lamps 18 are distributed in the interlayer cavity 17.
In order to improve the practicability of the product and facilitate the user to see the internal pressure value, the cover plate 5 is provided with a pressure gauge 51.
Preferably, the vortex impeller 8 comprises a blade rod 81 arranged on the rotating shaft 20, and the end of the blade rod 81 is provided with a vertical blade 82; the vertical blade 82 comprises a vertical plate 821 vertical to the horizontal plane, and an inclined plate 822 inclined to the horizontal plane is integrally arranged at the upper end of the vertical plate 821.
Preferably, the bottom surface of the inner cylinder 3 is provided with two layers, including a lower bottom plate 34 at the lower layer and a disc plate 32 at the upper layer; the edge of the disc plate 32 is uniformly provided with connecting rods 33 which are connected with the inner wall of the inner cylinder 3; the vortex impeller 8 is arranged between the lower bottom plate 34 and the disc plate 32; the disc plate 32 shields the blade bars 81.
Preferably, the barrel impeller 9 comprises an upper mounting ring 92 and a lower mounting ring 93; straight blades 91 are uniformly distributed between the upper mounting ring 92 and the lower mounting ring 93 in an annular manner; the lower mounting ring 93 is coaxially connected with the rotating shaft 20 through a mounting rod 94; the upper mounting ring 92 is mounted on the bottom surface of the top plate 7 by a bearing.
In order to facilitate the illumination and heat the material, the reflecting cover of the infrared heating tube 6 is conical.
The cover plate 5 is provided with a handle 52.
The inner wall 22 of the drying cylinder 2 is in a wave shape, so that the water vapor absorption area and the water vapor absorption efficiency of the drying cylinder 2 can be improved.
The invention specifically uses the principle:
start driving motor 46, driving motor 46 passes through drive gear and drives 47 rotations of chain, chain 47 drives pinion 48 rotatory, pinion 48 drives two vertical lead screw 49 rotations that mutual symmetry set up, when lead screw 49 is rotatory, it rises to drive apron 5, jib 43 of apron 5 lower extreme also follows and rises, the layer board 41 of placing on the jib 43 also follows and rises outside feed inlet 50, convenience of customers puts the material on layer board 41, then driving motor 46 counter rotation, at last apron 5 covers feed inlet 50, layer board 41 descends in the inner tube 3.
In order to improve the use flexibility of the device, the hanger rod 43 is evenly provided with positioning blocks 44, and the supporting plate 41 can be placed on the positioning blocks 44 with different heights on the hanger rod 43, so that the height of the supporting plate 41 can be adjusted.
Starting the infrared heating pipe 6, starting the motor 19 at the same time, the infrared heating pipe 6 performs illumination heating on the air in the inner barrel 3, the motor 19 drives the barrel type impeller 9, the exhaust fan blade 10 and the vortex impeller 8 to rotate, the vortex impeller 8 is stirred and rotated in the inner barrel 3, so that the air in the inner barrel 3 rotates at a high speed to form a vortex, when the stirring speed is up to a preset value, the air in the inner barrel 3 generates a tornado type vortex, and is heated by the infrared heating pipe 6 at the same time to form a thermal vortex, so that the air overflows to the periphery, the air pressure at the center of the inner barrel 3 is reduced, a certain negative pressure effect is formed, so that the water vapor in the material can be rapidly emitted and is thrown to the periphery, the water vapor and the air rotate at a high speed to be emitted, the water vapor and the air further push of the barrel type impeller 9 impact the inner, the drying agent is absorbed by the drying agent, the drying agent is generally a silica gel type physical drying agent, when the exhaust fan blade 10 rotates, a large negative pressure is formed in a cavity between the drying cylinder 2 and the outer cylinder 1, so that water vapor absorbed in the drying cylinder 2 is pumped out by the negative pressure, and then is discharged from an upper port of the interlayer cavity 17 through the interlayer cavity 17. Because the material is not the direct drying of the heat that receives the electrothermal resistance silk to produce in drying process, also not directly receive very big negative pressure and take out steam, therefore the drying process of material is steady and quick, and it is very little to the structure and the form influence of material itself, and the specially adapted pharmacy is used.
When the material is by the dry back, can control motor 19 reversal for outside air is reverse to enter into the equipment inner tube, makes inside atmospheric pressure resume normal fast, takes place the form change with the material, and convenience of customers opens equipment simultaneously, and the motor is at the reversal in-process, and outside cold air gets into the inside cooling rate that also can improve the material of equipment.
The supporting plate 41 is of a mesh structure and is hung by a sliding rod, so that the containing structure in the equipment cannot influence the effect of negative pressure heat vortexes, and the material can be stably and normally dried and dehumidified by the negative pressure heat vortexes.
The cylinder type impeller 9 can promote the generation of air vortexes in the rotating process, can improve the forming effect of negative pressure in the air vortexes, and has the effect of compressing water vapor to enter the drying cylinder.
Equipment is at the operation in-process, and 2 interior wall parts of drying cylinder receive high pressure atmospheric pressure effect, and in steam was extruded and entered into drying cylinder 2, 2 outer wall parts of drying cylinder received high negative pressure effect, steam can be absorbed out from the drier in drying cylinder 2 and is got rid of. The negative pressure intensity of the outer wall of the drying cylinder 2 is far greater than the negative pressure effect in the inner cylinder 3. The negative pressure effect in the inner cylinder 3 is not too high, so as to avoid influencing the change of the material form.
The vortex impeller 8 has the main functions that the air in the inner barrel 3 generates vortex to form tornado, so that the center of the vortex forms a local negative pressure effect, and the vertical blades 82 and the blade rods 81 are obliquely arranged instead of being arranged in parallel, so that the vortex impeller 8 has a certain exhaust effect, and the air is quickly dispersed to the periphery; the sloping plate 822 on the vertical blade 82 can enable the air to form a rising effect, so that water vapor in the material in the center can rise and overflow quickly, and the drying effect is improved.
When equipment corotation, it is rotatory to control air purification ring 74 earlier, exposes blow vent 72 for the air in the intermediate layer chamber 17 can be fast smooth and easy arrange the external world to go, and when equipment was about to the reversal or was about to stop, control air purification ring 74 was rotatory shelters from blow vent 72, makes the outside air when reverse entering equipment is inside, just can get into after need being filtered and purified, avoids outside pollutant to pollute by dry material.
Compared with the traditional heating by using an electric resistance wire, the infrared heating tube has the advantages of high thermal efficiency, high power density, rapid temperature rise, electricity saving and long service life, is an illumination type heating, and has small influence on intermediate products in the pharmaceutical process.
The disc plate 32 can shield the air swirl effect generated by the rotation of the blade rod 81, so that the air in the middle of the inner barrel 3 is in a relatively stable effect, the material cannot be subjected to a large air flow effect, the material is prevented from floating due to the swirl, the connecting rod 33 cannot shield the stirring effect of the vertical blade 82, the air around the inner barrel 3 forms a high-speed rotation effect, and the negative pressure effect generated when the tornado is formed in the inner barrel 3 in a simulated mode is achieved.
the following parts are volume parts, such as L, cube and the like, DMF is N, N-dimethylformamide, PTS is p-toluenesulfonic acid, monoester is 17 α -hydroxyprogesterone acetate, and hydrochloric acid concentration is 36% by mass;
process example one for the production of medroxyprogesterone acetate, which comprises the following steps:
preparation of acetic acid methine:
pumping 400 parts of tetrahydrofuran into a reaction kettle, adding 130 parts of 17 α -hydroxyprogesterone acetate, stirring, pumping 50 parts of triethyl orthoformate and 70 parts of absolute ethyl alcohol, introducing nitrogen, adding 2 parts of PTS, carrying out heat preservation reaction at 34-36 ℃ for 0.8 hour, adding 2 parts of PTS, reacting for 1 hour, reducing the temperature to 25-30 ℃, sequentially pumping 40 parts of N-methylaniline and 40 parts of formaldehyde, heating to 34-36 ℃ for reaction for 2 hours, pumping the reaction solution into a elutriation kettle, reducing the temperature to 10 ℃, dropwise adding 150 parts of hydrochloric acid, carrying out heat preservation reaction at 23-27 ℃ for 1 hour, slowly adding 1400 parts of water for elutriation, reducing the temperature to 4 ℃, stirring for 2 hours, centrifuging, washing to be neutral, putting into a drying device, starting an infrared heating pipe 6, irradiating for 8 minutes, controlling the rotating speed of a motor 19 to be 1000r/min, and continuously operating for 15 minutes to obtain acetic acid methine;
the reaction formula is as follows:
hydrogenation reaction:
pumping 400 parts of DMF (dimethyl formamide) into a reaction kettle, adding 130 parts of the acetic acid methine, introducing nitrogen, adding 20 parts of palladium-carbon and 50 parts of cyclohexene, heating to 96-100 ℃ for reaction for 2 hours, filtering to a transposition kettle, cooling the filtrate to 15 ℃, adding 15 parts of hydrochloric acid, keeping the temperature of 20-22 ℃ for 1 hour after the addition, adding 15 parts of sodium bicarbonate, cooling to 0 ℃, keeping the temperature for 2 hours after the addition, centrifuging, washing with water, spin-drying, and drying to obtain a crude product; adding 500 parts of dichloromethane, 800 parts of ethanol, 120 parts of the crude product and 12 parts of activated carbon into a decoloring kettle, heating to 35 ℃ for reflux, decoloring for 20 minutes, filtering paper concentrating the kettle, concentrating to a small volume, cooling to about 2V mother liquor, crystallizing for 1.5 hours at 0-5 ℃, centrifuging, spin-drying, putting into a drying device, starting an infrared heating pipe 6, irradiating for 8 minutes, controlling the rotating speed of a motor 19 to be 1300r/min, and continuously operating for 15 minutes to obtain a refined medroxyprogesterone acetate;
the reaction formula is as follows:
process example II for the production of medroxyprogesterone acetate, comprising the following steps:
another objective of the present invention is to provide a process for producing medroxyprogesterone acetate, which can shorten the production time of medroxyprogesterone acetate by using the above-mentioned production apparatus, comprising the following steps:
preparation of acetic acid methine:
pumping 500 parts of tetrahydrofuran into a reaction kettle, adding 170 parts of 17 α -hydroxyprogesterone acetate, stirring, pumping 70 parts of triethyl orthoformate and 90 parts of absolute ethyl alcohol, introducing nitrogen, adding 4 parts of PTS, carrying out heat preservation reaction at 34-36 ℃ for 1.5 hours, adding 4 parts of PTS, reacting for 2 hours, reducing the temperature to 30 ℃, sequentially pumping 50 parts of N-methylaniline and 50 parts of formaldehyde, heating to 34-36 ℃ for reaction for 3 hours, pumping the reaction solution into a elutriation kettle, cooling to 20 ℃, dropwise adding 200 parts of hydrochloric acid, carrying out heat preservation reaction at 23-27 ℃ for 2 hours, slowly adding 1600 parts of water for elutriation, cooling to 6 ℃, stirring for 4 hours, centrifuging, washing to be neutral, putting into a drying device, starting an infrared heating pipe 6, irradiating for 12 minutes, controlling the rotation speed of a motor 19 to be 1300r/min, and continuously operating for 10 minutes to obtain acetic acid methine;
hydrogenation reaction:
pumping 500 parts of DMF into a reaction kettle, adding 170 parts of the acetic acid methine, introducing nitrogen, adding 30 parts of palladium-carbon and 70 parts of cyclohexene, heating to 96-100 ℃ for reaction for 3 hours, filtering to a transposition kettle, cooling the filtrate to 25 ℃, adding 20 parts of hydrochloric acid, keeping the temperature of 20-22 ℃ for 2 hours, adding 20 parts of sodium bicarbonate, cooling to 0 ℃ after the addition, keeping the temperature for 4 hours, centrifuging, washing with water, spin-drying, and drying to obtain a crude product; adding 600 parts of dichloromethane, 820 parts of ethanol, 140 parts of the crude product and 14 parts of activated carbon into a decoloring kettle, heating to 45 ℃ for reflux, decoloring for 40 minutes, filtering paper concentrating the kettle, concentrating to a small volume, cooling to 0-5 ℃ for crystallization for 2.5 hours after about 2V of mother liquor, centrifuging, spin-drying, putting into the drying equipment, starting an infrared heating pipe 6, irradiating for 12 minutes, controlling the rotating speed of a motor 19 to be 500r/min, and continuously operating for 10 minutes to obtain the refined medroxyprogesterone acetate.
Third process example for producing medroxyprogesterone acetate, it includes the following steps:
preparation of acetic acid methine:
pumping 450 parts of tetrahydrofuran into a reaction kettle, adding 150 parts of 17 α -hydroxyprogesterone acetate, stirring, pumping 60 parts of triethyl orthoformate and 80 parts of absolute ethyl alcohol, introducing nitrogen, adding 3 parts of PTS, carrying out heat preservation reaction at 34-36 ℃ for 1 hour, adding 3 parts of PTS, carrying out reaction for 1.5 hours, reducing the temperature to 28 ℃, sequentially pumping 45 parts of N-methylaniline and 45 parts of formaldehyde, heating to 34-36 ℃ for 2.5 hours, pumping the reaction liquid into a elutriation kettle, reducing the temperature to 15 ℃, dropwise adding 180 parts of hydrochloric acid, completing dropwise addition within 30 minutes, carrying out heat preservation reaction at 23-27 ℃ for 1.5 hours, slowly adding 1500 parts of elutriation, reducing the temperature to 5 ℃, stirring for 3 hours, centrifuging, washing to be neutral, putting into the drying equipment, starting an infrared heating pipe 6, irradiating for 8-12 minutes, controlling the rotation speed of a motor 19 to be 1000-1300r/min, and continuously operating for 10-15 minutes to obtain acetic acid methine;
hydrogenation reaction:
pumping 450 parts of DMF into a reaction kettle, adding 150 parts of the acetic acid methine, introducing nitrogen, adding 24 parts of palladium-carbon and 60 parts of cyclohexene, heating to 96-100 ℃, reacting for 2 hours and 40 minutes, filtering to a transposition kettle, cooling the filtrate to 20 ℃, adding 18 parts of hydrochloric acid, preserving heat for 1.5 hours at 20-22 ℃, adding 18 parts of sodium bicarbonate, cooling to 0 ℃ after adding, preserving heat for 3 hours, centrifuging, washing with water, spin-drying, and drying to obtain a crude product; adding 540 parts of dichloromethane, 810 parts of ethanol, 135 parts of the crude product and 13.5 parts of activated carbon into a decoloring kettle, heating and refluxing (at 40 ℃) for decoloring for 30 minutes, concentrating the filtrate in a filter paper concentrating kettle to a small volume, cooling to about 2V of mother liquor, crystallizing for 2 hours at 0-5 ℃, centrifuging, spin-drying, putting into the drying equipment, starting an infrared heating pipe 6, irradiating for 8-12 minutes, controlling the rotating speed of a motor 19 to be 1300-1500r/min, and continuously operating for 10-15 minutes to obtain the refined medroxyprogesterone acetate.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts of the present invention. The foregoing is only a preferred embodiment of the present invention, and it should be noted that there are objectively infinite specific structures due to the limited character expressions, and it will be apparent to those skilled in the art that a plurality of modifications, decorations or changes may be made without departing from the principle of the present invention, and the technical features described above may be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments.
Claims (10)
1. A medroxyprogesterone acetate production device comprises a reaction kettle, a elutriation kettle, a centrifugal machine, a concentration kettle, a decoloration kettle and drying equipment which are connected with each other according to working procedures, and is characterized in that the drying equipment comprises an outer cylinder (1), a drying cylinder (2) is coaxially arranged in the outer cylinder (1), and an inner cylinder (3) is coaxially arranged in the drying cylinder (2); the upper ends of the outer cylinder (1), the drying cylinder (2) and the inner cylinder (3) are connected with a top plate (7); a motor (19) is arranged in the center of the bottom surface of the outer cylinder (1), and a rotating shaft (20) at the top end of the motor (19) extends into the inner cylinder (3); the exhaust fan blades (10), the cylindrical impeller (9) and the vortex impeller (8) are sequentially arranged on the rotating shaft (20) from bottom to top; the exhaust fan blades (10) are arranged between the bottom surface (24) of the drying cylinder and the bottom surface of the outer cylinder (1); the cylinder type impeller (9) is arranged between the drying cylinder (2) and the inner cylinder (3); the vortex impeller (8) is arranged at the bottom of the inner barrel (3); the top surface of the inner cylinder (3) is provided with an annular infrared heating pipe (6); the side wall of the drying cylinder (2) is a double-layer mesh plate, and a drying agent (22) is filled in an interlayer of the double-layer mesh plate; the side wall of the inner cylinder (3) is a mesh plate; the side wall of the outer cylinder (1) comprises an inner layer wall (11) and an outer layer wall (12); an interlayer cavity (17) is formed between the inner layer wall (11) and the outer layer wall (12); the lower end of the inner wall (11) is provided with an exhaust hole (26) communicated with the interlayer cavity (17); an annular baffle (71) is arranged at an outlet at the upper end of the interlayer cavity (17); vent holes (72) are uniformly arranged on the baffle plate (71) in a ring shape; the upper end of the baffle (71) is provided with a rotatable air purification ring (74); an air filter (73) for shielding the air vent (72) is arranged on the air purification ring (74); a feed inlet (50) is formed in the center of the top plate (7), and an inverted U-shaped bracket (45) is arranged above the feed inlet (50); screw rods (49) connected with a driving motor (46) are arranged on two sides in the bracket (45); the screw rod (49) is provided with a cover plate (5) capable of lifting up and down; a hanging rod (43) is vertically arranged at the lower end of the cover plate (5), and positioning blocks (44) used for supporting the supporting plate (41) are uniformly arranged on the hanging rod (43); the support plate (41) is horizontally arranged between the suspension rods (43).
2. The medroxyprogesterone acetate production device according to claim 1, wherein the driving motor (46) is arranged at the top end of the bracket (45); a pinion (48) is arranged at the upper end of the screw rod (49); the pinion (48) is connected with a driving gear on the driving motor (46) through a chain (47).
3. The medroxyprogesterone acetate production device according to claim 1, wherein four suspension rods (43) are arranged at the lower end of the cover plate () 5 and are distributed in a rectangular shape; the bottom end of the hanging rod (43) is connected with a fixed frame (42).
4. The medroxyprogesterone acetate production device according to claim 1, wherein ultraviolet lamps (18) are distributed in the interlayer cavity (17).
5. The medroxyprogesterone acetate production device according to claim 1, wherein the vortex impeller (8) comprises a blade rod (81) arranged on the rotating shaft (20), and the end of the blade rod (81) is provided with a vertical blade (82); the vertical blade (82) comprises a vertical plate (821) vertical to the horizontal plane, and an inclined plate (822) inclined to the horizontal plane is integrally arranged at the upper end of the vertical plate (821).
6. The medroxyprogesterone acetate production device according to claim 5, characterized in that the bottom surface of the inner cylinder (3) is provided with two layers, including a lower bottom plate (34) at the lower layer and a disc plate (32) at the upper layer; the edge of the disc plate (32) is uniformly provided with connecting rods (33) which are connected with the inner wall of the inner cylinder (3); the vortex impeller (8) is arranged between the lower bottom plate (34) and the disc plate (32); the disc plate (32) shields the blade rods (81).
7. Medroxyprogesterone acetate production device according to claim 1, characterized in that said barrel impeller (9) comprises an upper mounting ring (92) and a lower mounting ring (93); straight blades (91) are uniformly distributed between the upper mounting ring (92) and the lower mounting ring (93) in an annular manner; the lower mounting ring (93) is coaxially connected with the rotating shaft (20) through a mounting rod (94); the upper mounting ring (92) is arranged on the bottom surface of the top plate (7) through a bearing.
8. The medroxyprogesterone acetate production device according to claim 1, wherein the reflector of the infrared heating tube (6) is conical.
9. A process for the manufacture of medroxyprogesterone acetate using an medroxyprogesterone acetate manufacturing apparatus according to any of claims 1 to 8, comprising the steps of:
preparation of acetic acid methine:
pumping 400-500 parts of tetrahydrofuran into a reaction kettle, adding 130-170 parts of 17 α -hydroxyprogesterone acetate, stirring, pumping 50-70 parts of triethyl orthoformate and 70-90 parts of absolute ethyl alcohol, introducing nitrogen, adding 2-4 parts of PTS, carrying out heat preservation reaction at 34-36 ℃ for 0.8-1.5 hours, adding 2-4 parts of PTS, reacting for 1-2 hours, cooling to 25-30 ℃, sequentially pumping 40-50 parts of N-methylaniline and 40-50 parts of formaldehyde, heating to 34-36 ℃ for reaction for 2-3 hours, pumping the reaction liquid into a elutriation kettle, cooling to 10-20 ℃, dropwise adding 150-200 parts of hydrochloric acid, carrying out heat preservation reaction at 23-27 ℃ for 1-2 hours, slowly adding 1400-1600 parts of water for elutriation, cooling to 4-6 ℃, stirring for 2-4 hours, centrifuging, washing to be neutral, putting into a drying device, starting an infrared heating pipe (6) for irradiation, controlling the rotation speed of a motor (19) to be 1000-1300r/min, continuously operating for 10-15 minutes, and obtaining methyl acetate;
the reaction formula is as follows:
hydrogenation reaction:
pumping 400-500 parts of DMF (dimethyl formamide) into a reaction kettle, adding 130-170 parts of the acetic acid methine, introducing nitrogen, adding 20-30 parts of palladium carbon and 50-70 parts of cyclohexene, heating to 96-100 ℃ for reaction for 2-3 hours, filtering to a transposition kettle, cooling the filtrate to 15-25 ℃, adding 15-20 parts of hydrochloric acid, keeping the temperature for 1-2 hours at 20-22 ℃ after the addition is finished, adding 15-20 parts of sodium bicarbonate, cooling to 0 ℃ after the addition is finished, keeping the temperature for 2-4 hours, centrifuging, washing with water, spin-drying, and drying to obtain a crude product; adding 500-600 parts of dichloromethane, 800-820 parts of ethanol, 120-140 parts of the crude product and 12-14 parts of activated carbon into a decoloring kettle, heating to 35-45 ℃ for reflux, decoloring for 20-40 minutes, concentrating the filtrate in a filter paper concentrating kettle to a small volume of about 2V mother liquor, cooling to 0-5 ℃ for crystallization for 1.5-2.5 hours, centrifuging and spin-drying, putting the product into a drying device, starting an infrared heating pipe (6), irradiating for 8-12 minutes, controlling the rotating speed of a motor (19) to be 1300-1500r/min, and continuously operating for 10-15 minutes to obtain a refined medroxyprogesterone acetate product;
the reaction formula is as follows:
10. the process for producing medroxyprogesterone acetate according to claim 9, comprising the following steps:
preparation of acetic acid methine:
pumping 450 parts of tetrahydrofuran into a reaction kettle, adding 150 parts of 17 α -hydroxyprogesterone acetate, stirring, pumping 60 parts of triethyl orthoformate and 80 parts of absolute ethyl alcohol, introducing nitrogen, adding 3 parts of PTS, carrying out heat preservation reaction at 34-36 ℃ for 1 hour, adding 3 parts of PTS, carrying out reaction for 1.5 hours, reducing the temperature to 28 ℃, sequentially pumping 45 parts of N-methylaniline and 45 parts of formaldehyde, heating to 34-36 ℃ for 2.5 hours, pumping the reaction liquid into a elutriation kettle, reducing the temperature to 15 ℃, dropwise adding 180 parts of hydrochloric acid, completing dropwise addition within 30 minutes, carrying out heat preservation reaction at 23-27 ℃ for 1.5 hours, slowly adding 1500 parts of elutriation, reducing the temperature to 5 ℃, stirring for 3 hours, centrifuging, washing to be neutral, putting into the drying equipment, starting an infrared heating pipe (6), irradiating for 8-12 minutes, controlling the rotating speed of a motor (19) to be 1000-1300r/min, and continuously operating for 10-15 minutes to obtain acetic acid methine;
hydrogenation reaction:
pumping 450 parts of DMF into a reaction kettle, adding 150 parts of the acetic acid methine, introducing nitrogen, adding 24 parts of palladium-carbon and 60 parts of cyclohexene, heating to 96-100 ℃, reacting for 2 hours and 40 minutes, filtering to a transposition kettle, cooling the filtrate to 20 ℃, adding 18 parts of hydrochloric acid, preserving heat for 1.5 hours at 20-22 ℃, adding 18 parts of sodium bicarbonate, cooling to 0 ℃ after adding, preserving heat for 3 hours, centrifuging, washing with water, spin-drying, and drying to obtain a crude product; adding 540 parts of dichloromethane, 810 parts of ethanol, 135 parts of the crude product and 13.5 parts of activated carbon into a decoloring kettle, heating to 40 ℃ for reflux, decoloring for 30 minutes, filtering paper concentrating the kettle, concentrating to a small volume, cooling to 0-5 ℃ for crystallization for 2 hours, centrifuging, spin-drying, putting into a drying device, starting an infrared heating pipe (6), irradiating for 8-12 minutes, controlling the rotating speed of a motor (19) to be 1300-1500r/min, and continuously operating for 10-15 minutes to obtain the refined medroxyprogesterone acetate.
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| CN109627277A (en) * | 2018-12-19 | 2019-04-16 | 上海新华联制药有限公司 | A kind of preparation method of medroxyprogesterone acetate |
| US11713923B2 (en) * | 2021-02-03 | 2023-08-01 | Marthinus Jacobus Bekker | Horizontal surface dryer |
| CN114057821B (en) * | 2021-11-30 | 2022-12-09 | 黑龙江中医药大学 | Preparation method of medroxyprogesterone acetate for perimenopausal syndrome |
| CN115388624B (en) * | 2022-08-30 | 2023-06-13 | 湖南越洋药业有限公司 | Rotary adjustable drying equipment applied to methylprednisolone production |
| CN115388625B (en) * | 2022-08-30 | 2023-06-13 | 湖南越洋药业有限公司 | Backflushing rotary type drying equipment applied to methylprednisolone production |
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