CN108912191B - Estradiol production process and production device - Google Patents
Estradiol production process and production device Download PDFInfo
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- CN108912191B CN108912191B CN201810826705.7A CN201810826705A CN108912191B CN 108912191 B CN108912191 B CN 108912191B CN 201810826705 A CN201810826705 A CN 201810826705A CN 108912191 B CN108912191 B CN 108912191B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J1/00—Normal steroids containing carbon, hydrogen, halogen or oxygen, not substituted in position 17 beta by a carbon atom, e.g. estrane, androstane
- C07J1/0051—Estrane derivatives
- C07J1/0066—Estrane derivatives substituted in position 17 beta not substituted in position 17 alfa
- C07J1/007—Estrane derivatives substituted in position 17 beta not substituted in position 17 alfa the substituent being an OH group free esterified or etherified
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
- F26B23/04—Heating arrangements using electric heating
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Abstract
The invention discloses an estradiol 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 formed in the center of the top plate, a slide bar is arranged at the edge of the feed inlet, and the lower end of the slide bar is connected with a tray; a screw rod is arranged on the side edge of the feeding hole, a screw sleeve is arranged on the screw rod, a gear ring is arranged on the screw sleeve and is meshed with a driving gear, and the driving gear is connected with a driving motor; the lower end of the screw rod is connected with the tray; the top ends of the slide rod and the screw rod are connected with a cover plate. The invention can reduce the preparation time of the intermediate product in the estradiol production process and realize the rapid high-quality production of the estradiol.
Description
Technical Field
The invention belongs to the technical field of medicine production, and particularly relates to a process and a device for producing estradiol.
Background
the traditional estradiol is produced by adopting multi-step chemical reaction, and the formed intermediate product raw material needs 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 great negative influence on the intermediate product for preparing the estradiol, so that the structure of the intermediate product is changed, the subsequent estradiol crystallization is unstable, the purity is reduced, meanwhile, the drying time is long regardless of the existing electrothermal filament heating drying equipment or the existing vacuum pumping negative pressure dehumidification equipment, the vacuum pumping negative pressure dehumidification can realize quick dehumidification by adopting a quick pressure reduction mode, but the quick pressure reduction easily causes the variation of the shape and the structure of the intermediate product, and the subsequent estradiol production quality is reduced.
Disclosure of Invention
The invention aims to solve the problems and provides an estradiol production device, which adopts drying equipment to be flexibly adjusted, can form a gentle local vortex type thermal negative pressure effect, does not damage the material structure, can quickly dry, reduces the preparation time of an intermediate product in the estradiol production process, and realizes the quick high-quality production of estradiol.
In order to realize the purpose, the invention adopts the technical scheme that: an estradiol production device comprises a reaction kettle, a elutriation kettle, a centrifugal machine, a concentration kettle, a decoloring kettle and drying equipment which are connected with each other according to working procedures, wherein the drying equipment 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, two slide bars capable of lifting up and down are symmetrically arranged on the edge of the feed inlet, and the lower ends of the slide bars are connected to the two sides of the tray; a screw rod is arranged on the side edge of the feeding hole, a screw sleeve is arranged on the screw rod, a gear ring is arranged on the screw sleeve and is meshed with a driving gear, and the driving gear is connected with a driving motor; the lower end of the screw rod is connected with the edge of the tray; the top ends of the sliding rods and the screw rods are connected with a cover plate.
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 object of the present invention is to provide a process for producing estradiol, which can shorten the production time of estradiol by using the above-mentioned production apparatus, comprising the steps of:
preparation of ketal:
pumping 160-200 parts of ethylene glycol and 130-170 parts of triethyl orthoformate into a reaction kettle, adding 2-4 parts of p-toluenesulfonic acid and 130-170 parts of 1, 4-androstenedione, controlling the temperature to be 15-20 ℃, preserving heat for reaction for 2-4 hours, adding triethylamine to adjust p H-4, adding water for precipitation, centrifuging, washing to be neutral, putting into drying equipment, starting an infrared heating pipe, irradiating for 8-12 minutes, controlling the rotating speed of a motor to be 1000-1300r/min, and continuously operating for 10-15 minutes to form a ketal compound;
the reaction formula is as follows:
aromatization hydrolysis reaction:
adding 1600-1700 parts of tetrahydrofuran, 45-55 parts of biphenyl, 60-70 parts of diphenylmethane and nitrogen into a reaction kettle, adjusting the temperature to 35-40 ℃, adding 7-9 parts of lithium particles, continuing to stir at 40-50 ℃ for 30 minutes, cooling to 20-25 ℃, adding 150-170 parts of the ketal, reacting at 36-40 ℃ for 2 hours, cooling to below 10 ℃, dropwise adding 450-500 parts of methanol, controlling the temperature to be less than 35 ℃, adding 150-170 parts of hydrochloric acid, adjusting p H = 3-4, refluxing for 2 hours, after the reaction is finished, concentrating under reduced pressure to be solvent-free, centrifuging, washing with water, spin-drying, putting into a drying device, starting an infrared heating pipe, irradiating for 6-10 minutes, controlling the rotating speed of a motor to be 1100-1300r/min, and continuously operating for 12-18 minutes to form a hydrolysate crude product;
pumping 1000-1100 parts of ethanol into a refining kettle, adding 100-110 parts of the hydrolysate crude product and 7-9 parts of activated carbon, heating and refluxing for 30 minutes, filtering, concentrating under reduced pressure to about 3 times of volume of mother liquor, cooling to below 5 ℃, centrifuging, spin-drying, adding into the drying equipment, starting an infrared heating pipe, irradiating for 10-15 minutes, controlling the rotating speed of a motor to be 1200-1500r/min, and continuously operating for 13-20 minutes to obtain a hydrolysate fine product;
the reaction formula is as follows:
reduction reaction and refining:
pumping 1000-1100 parts of methanol into a reaction kettle, adding the hydrolysate refined product, stirring, cooling to 0-5 ℃, adding 9-10 parts of potassium borohydride for reaction for 4-5 hours, adding glacial acetic acid for neutralization until p H is 7, heating to 50-60 ℃, carrying out negative pressure concentration on the methanol, adding water for elutriation, carrying out centrifugal drying, putting into a drying device, starting an infrared heating pipe, irradiating for 4-6 minutes, controlling the rotating speed of a motor to be 1200-1500r/min, and continuously operating for 8-12 minutes to obtain an estradiol crude product;
pumping 1100-1200 parts of methanol into a decoloring kettle, adding 90-100 parts of the estradiol crude product, heating to 60-65 ℃, adding 8-10 parts of activated carbon, decoloring for 1-3 hours, filtering to a crystallization kettle, reducing the pressure to 0-5 ℃ until the residual amount of mother liquor is 2 times of the weight of the product, crystallizing for 1.5-2.5 hours, centrifuging, spin-drying, putting into a drying device, starting an infrared heating pipe, irradiating for 8-12 minutes, controlling the rotating speed of a motor to be 1200-1500r/min, and continuously operating for 12-18 minutes to obtain an estradiol refined product;
the reaction formula is as follows:
a preferred process for producing estradiol comprises the following preparation steps:
preparation of ketal:
pumping 180 parts of ethylene glycol and 150 parts of triethyl orthoformate into a reaction kettle, adding 3 parts of p-toluenesulfonic acid and 150 parts of 1, 4-androstenedione, controlling the temperature to be 15-20 ℃, carrying out heat preservation reaction for 3 hours, adding triethylamine, adjusting p H-3.8 drops, adding 900 parts of water, carrying out precipitation, centrifuging, washing to be neutral, putting into drying equipment, starting an infrared heating pipe, irradiating for 10 minutes, controlling the rotating speed of a motor to be 1000-1300r/min, and continuously operating for 12 minutes to form a ketal;
the aromatization hydrolysis reaction is carried out,
adding 1620 parts of tetrahydrofuran, 50 parts of biphenyl, 65 parts of diphenylmethane and nitrogen into a reaction kettle, adjusting the temperature to 35-40 ℃, adding 8.1 parts of lithium particles, continuing to stir at 40-50 ℃ for 30 minutes, cooling to 20-25 ℃, adding 162 parts of the ketal, reacting at 36-40 ℃ for 2 hours at a stirring temperature of less than or equal to 40 ℃, slowly dripping 486 parts of methanol at a temperature of less than 35 ℃, adding 162 parts of hydrochloric acid solution, adjusting p H = 3-4, heating, refluxing for 2 hours, concentrating under reduced pressure until no solvent exists after the reaction is finished, centrifuging, washing with water, spin-drying, putting into a drying device, starting an infrared heating pipe, irradiating for 8 minutes, controlling the rotating speed of a motor to be 1100-1300r/min, and continuously operating for 15 minutes to form a hydrolysate crude product;
pumping 1050 parts of ethanol into a refining kettle, adding 105 parts of the hydrolysate crude product and 8 parts of activated carbon, heating and refluxing for 30 minutes, filtering, concentrating under reduced pressure to about 3 times of volume of mother liquor, cooling to below 5 ℃, centrifuging, spin-drying, putting into the drying equipment, starting an infrared heating pipe, irradiating for 12 minutes, controlling the rotating speed of a motor to be 1200-1500r/min, and continuously operating for 15 minutes to obtain a hydrolysate fine product;
reduction reaction and refining:
pumping 1060 parts of methanol into a reaction kettle, adding the hydrolysate refined product, stirring, cooling to 0-5 ℃, adding 9.6 parts of potassium borohydride by times for reaction for 4-5 hours, adding glacial acetic acid for neutralization until p H is 7, heating to 50-60 ℃, concentrating the methanol under negative pressure, adding water for elutriation, centrifugally drying, putting into a drying device, starting an infrared heating pipe, irradiating for 5 minutes, controlling the rotation speed of a motor to be 1200-1500r/min, and continuously operating for 10 minutes to obtain an estradiol crude product;
pumping 1140 parts of methanol into a decoloring kettle, adding 95 parts of the estradiol crude product, heating to 60-65 ℃, adding 9 parts of activated carbon, decoloring for 2 hours, filtering to a crystallization kettle, performing negative pressure until the residual amount of mother liquor is 2 times of the weight of the product, cooling to 0-5 ℃ for crystallization for 2 hours, centrifuging, spin-drying, putting into a drying device, starting an infrared heating pipe, irradiating for 10 minutes, controlling the rotating speed of a motor to be 1200-1500r/min, and continuously operating for 15 minutes to obtain the estradiol refined product.
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 estradiol is shortened by about 30 percent, and the yield is improved by 20 to 30 percent.
2. The tray in the drying equipment can be automatically lifted to the position of the feeding hole, so that a user can conveniently put materials in and take out the materials, and meanwhile, the cover plate can be automatically opened and closed, so that the operation convenience of the equipment is 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 shape of the material is very small, the shape and the structure of an intermediate product are ensured, and the subsequent production quality of the estradiol 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 estradiol production according to the present 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 an enlarged structural diagram of a part B in fig. 2.
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 tray; 42. a screw rod; 43. a slide bar; 44. sleeving the silk; 45. a gear ring; 46. a drive gear; 47. a drive motor; 48. 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 13, 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 48 is formed in the center of the top plate 7, two slide rods 43 capable of ascending and descending are symmetrically arranged on the edge of the feed inlet 48, and the lower ends of the slide rods 43 are connected to two sides of the tray 41; a screw rod 42 is arranged on the side edge of the feeding hole 48, a screw sleeve 44 is arranged on the screw rod 42, a gear ring 45 arranged on the screw sleeve 44 is meshed with a driving gear 46, and the driving gear 46 is connected with a driving motor 47; the lower end of the screw rod 42 is connected with the edge of the tray 41; the top ends of the sliding rod 43 and the screw rod 42 are connected with the cover plate 5.
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:
the driving motor 47 is started, the driving motor 47 drives the driving gear 46 to rotate, the driving gear 46 drives the screw sleeve 44 to rotate, the screw sleeve 44 drives the screw rod 42 to ascend, the screw rod 42 drives the sliding rod 43, the tray 41 and the cover plate 5 to ascend simultaneously, the tray 41 ascends to the position of the feed port 48, a user can conveniently place materials on the tray 41, then the driving motor 47 is controlled to overturn, and the cover plate 5 and the tray 41 descend simultaneously until the cover plate 5 seals the feed port 48.
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 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 parts by volume, such as L, cube and the like, and DMF is N, N-dimethylformamide; PTS is p-toluenesulfonic acid.
Process example one for the production of estradiol, comprising the following preparation steps:
preparation of ketal:
pumping 160 parts of ethylene glycol and 130 parts of triethyl orthoformate into a reaction kettle, adding 2 parts of p-toluenesulfonic acid and 130 parts of 1, 4-androstenedione, controlling the temperature to be 15-20 ℃, carrying out heat preservation reaction for 2 hours, adding triethylamine to adjust p H-3, adding water to separate out, centrifuging, washing with water to be neutral, putting into drying equipment, 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 form a ketal;
the reaction formula is as follows:
aromatization hydrolysis reaction:
adding 1700 parts of tetrahydrofuran, 55 parts of biphenyl, 70 parts of diphenylmethane and nitrogen into a reaction kettle, adjusting the temperature to 35-40 ℃, adding lithium particles, continuously stirring at 40-50 ℃ for 30 minutes, cooling to 20-25 ℃, adding 150 parts of the ketal, reacting at 36-40 ℃ for 2 hours, cooling to below 10 ℃, dropwise adding 450 parts of methanol, controlling the temperature to be lower than 35 ℃, adding 150 parts of hydrochloric acid, adjusting p H = 3-4, refluxing for 2 hours, concentrating under reduced pressure until no solvent exists after the reaction is finished, centrifuging, washing with water, spin-drying, putting into drying equipment, starting an infrared heating pipe 6, irradiating for 6 minutes, controlling the rotating speed of a motor 19 to be 1100r/min, and continuously operating for 18 minutes to form a hydrolysate crude product;
pumping 1000 parts of ethanol into a refining kettle, adding 100 parts of the hydrolysate crude product and 7 parts of activated carbon, heating and refluxing for 30 minutes, filtering, concentrating under reduced pressure to about 3 times of volume of mother liquor, cooling to below 5 ℃, centrifuging, spin-drying, putting into the drying equipment, starting an infrared heating pipe 6, irradiating for 10 minutes, controlling the rotating speed of a motor 19 to be 1200r/min, and continuously operating for 20 minutes to obtain a hydrolysate fine product;
the reaction formula is as follows:
reduction reaction and refining:
pumping 1000 parts of methanol into a reaction kettle, adding the hydrolysate refined product, stirring, cooling to 0-5 ℃, adding 9 parts of potassium borohydride for reaction for 4-5 hours, adding glacial acetic acid for neutralization until p H is 7, heating to 50-60 ℃, carrying out negative pressure concentration on the methanol, adding water for elutriation, carrying out centrifugal drying, putting into a drying device, starting an infrared heating pipe 6, irradiating for 4 minutes, controlling the rotating speed of a motor 19 to be 1200r/min, and continuously operating for 12 minutes to obtain an estradiol crude product;
pumping 1100 parts of methanol into a decoloring kettle, adding 90 parts of the estradiol crude product, heating to 60-65 ℃, adding 8 parts of activated carbon, decoloring for 1 hour, filtering to a crystallization kettle, performing negative pressure until the residual amount of mother liquor is 2 times of the weight of the product, reducing to 0-5 ℃ for crystallization for 1.5-2.5 hours, centrifuging, spin-drying, putting into the drying equipment, starting an infrared heating pipe 6, irradiating for 8 minutes, controlling the rotating speed of a motor 19 to be 1200r/min, and continuously operating for 18 minutes to obtain an estradiol refined product;
the reaction formula is as follows:
process example II for the production of estradiol, comprising the following preparation steps:
preparation of ketal:
pumping 200 parts of ethylene glycol and 170 parts of triethyl orthoformate into a reaction kettle, adding 4 parts of p-toluenesulfonic acid and 170 parts of 1, 4-androstenedione, controlling the temperature to be 15-20 ℃, carrying out heat preservation reaction for 4 hours, adding triethylamine to adjust p H-4, adding water to precipitate, centrifuging, washing with water to be neutral, putting into a drying device, starting an infrared heating pipe 6, irradiating for 12 minutes, controlling the rotating speed of a motor 19 to be 1300r/min, and continuously operating for 10 minutes to form a ketal;
aromatization hydrolysis reaction:
adding 1700 parts of tetrahydrofuran, 55 parts of biphenyl, 70 parts of diphenylmethane and nitrogen into a reaction kettle, adjusting the temperature to 35-40 ℃, adding 9 parts of lithium particles, continuing to stir at 40-50 ℃ for 30 minutes, cooling to 20-25 ℃, adding 170 parts of the ketal, reacting at 36-40 ℃ for 2 hours, cooling to below 10 ℃, dropwise adding 500 parts of methanol, controlling the temperature to be lower than 35 ℃, adding 170 parts of hydrochloric acid, adjusting p H = 3-4, refluxing for 2 hours, concentrating under reduced pressure until no solvent exists after the reaction is finished, centrifuging, washing with water, spin-drying, putting into the drying equipment, starting an infrared heating pipe 6, irradiating for 10 minutes, controlling the rotating speed of a motor 19 to be 1300r/min, and continuously operating for 12 minutes to form a hydrolysate crude product;
pumping 1100 parts of ethanol into a refining kettle, adding 110 parts of the hydrolysate crude product and 9 parts of activated carbon, heating and refluxing for 30 minutes, filtering, concentrating under reduced pressure to about 3 times of volume of mother liquor, cooling to below 5 ℃, centrifuging, spin-drying, putting into the drying equipment, starting an infrared heating pipe 6, irradiating for 15 minutes, controlling the rotating speed of a motor 19 to be 1500r/min, and continuously operating for 13 minutes to obtain a hydrolysate fine product;
reduction reaction and refining:
pumping 1100 parts of methanol into a reaction kettle, adding the hydrolysate refined product, stirring, cooling to 0-5 ℃, adding 10 parts of potassium borohydride for reaction for 4-5 hours, adding glacial acetic acid for neutralization until p H is 7, heating to 50-60 ℃, carrying out negative pressure concentration on the methanol, adding water for elutriation, carrying out centrifugal drying, putting into a drying device, starting an infrared heating pipe 6, irradiating for 6 minutes, controlling the rotating speed of a motor 19 to be 1500r/min, and continuously operating for 8 minutes to obtain an estradiol crude product;
pumping 1200 parts of methanol into a decoloring kettle, adding 100 parts of the estradiol crude product, heating to 60-65 ℃, adding 10 parts of activated carbon, decoloring for 3 hours, filtering to a crystallization kettle, performing negative pressure until the residual amount of mother liquor is 2 times of the weight of the product, cooling to 0-5 ℃ for 2.5 hours of crystallization, centrifuging, spin-drying, putting into a drying device, starting an infrared heating pipe 6, irradiating for 12 minutes, controlling the rotating speed of a motor 19 to be 1500r/min, and continuously operating for 12 minutes to obtain the estradiol refined product.
The third process example for producing estradiol comprises the following preparation steps:
preparation of ketal:
pumping 180 parts of ethylene glycol and 150 parts of triethyl orthoformate into a reaction kettle, adding 3 parts of p-toluenesulfonic acid and 150 parts of 1, 4-androstenedione, controlling the temperature to be 15-20 ℃, carrying out heat preservation reaction for 3 hours, adding triethylamine, adjusting p H-3.8 drops, adding 900 parts of water, carrying out precipitation, centrifuging, washing to be neutral, putting into drying equipment, starting an infrared heating pipe 6, irradiating for 10 minutes, controlling the rotating speed of a motor 19 to be 1000-1300r/min, and continuously operating for 12 minutes to form a ketal;
the aromatization hydrolysis reaction is carried out,
adding 1620 parts of tetrahydrofuran, 50 parts of biphenyl, 65 parts of diphenylmethane and nitrogen into a reaction kettle, adjusting the temperature to 35-40 ℃, adding 8.1 parts of lithium particles, continuing to stir at 40-50 ℃ for 30 minutes, cooling to 20-25 ℃, adding 162 parts of the ketal, reacting at 36-40 ℃ for 2 hours at a stirring temperature of less than or equal to 40 ℃, slowly dripping 486 parts of methanol, controlling the temperature to be less than 35 ℃, adding 162 parts of hydrochloric acid solution, adjusting p H = 3-4, heating, refluxing for 2 hours, concentrating under reduced pressure until no solvent exists after the reaction is finished, centrifuging, washing with water, 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 1100-1300r/min, and continuously operating for 15 minutes to form a hydrolysate crude product;
pumping 1050 parts of ethanol into a refining kettle, adding 105 parts of the hydrolysate crude product and 8 parts of activated carbon, heating and refluxing for 30 minutes, filtering, concentrating under reduced pressure to about 3 times of volume of mother liquor, cooling to below 5 ℃, 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 1200-1500r/min, and continuously operating for 15 minutes to obtain a hydrolysate fine product;
reduction reaction and refining:
pumping 1060 parts of methanol into a reaction kettle, adding the hydrolysate refined product, stirring, cooling to 0-5 ℃, adding 9.6 parts of potassium borohydride by times for reaction for 4-5 hours, adding glacial acetic acid for neutralization until p H is 7, heating to 50-60 ℃, concentrating the methanol under negative pressure, adding water for elutriation, centrifugally drying, putting into a drying device, starting an infrared heating pipe 6, irradiating for 5 minutes, controlling the rotation speed of a motor 19 to be 1200-1500r/min, and continuously operating for 10 minutes to obtain an estradiol crude product;
pumping 1140 parts of methanol into a decoloring kettle, adding 95 parts of the estradiol crude product, heating to 60-65 ℃, adding 9 parts of activated carbon, decoloring for 2 hours, filtering to a crystallization kettle, controlling the temperature to 55-65 ℃, controlling the negative pressure until the residual amount of the mother liquor is 2 times of the weight of the product, reducing the temperature to 0-5 ℃ for 2 hours of crystallization, centrifuging, spin-drying, putting into the drying equipment, starting an infrared heating pipe 6, irradiating for 10 minutes, controlling the rotating speed of a motor 19 to be 1200-1500r/min, and continuously operating for 15 minutes to obtain the estradiol refined product.
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. An estradiol production device comprises a reaction kettle, a elutriation kettle, a centrifugal machine, a concentration kettle, a decolorization kettle and drying equipment which are mutually connected 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 (48) is formed in the center of the top plate (7), two slide rods (43) capable of lifting up and down are symmetrically arranged on the edge of the feed inlet (48), and the lower ends of the slide rods (43) are connected to the two sides of the tray (41); a screw rod (42) is arranged on the side edge of the feeding hole (48), a screw sleeve (44) is arranged on the screw rod (42), a gear ring (45) is arranged on the screw sleeve (44) and meshed with a driving gear (46), and the driving gear (46) is connected with a driving motor (47); the lower end of the screw rod (42) is connected with the edge of the tray (41); the top ends of the sliding rod (43) and the screw rod (42) are connected with the cover plate (5).
2. Estradiol production device according to claim 1, characterized in that the inner wall of the inner wall (11) is distributed with infrared heating lamps (16).
3. Estradiol production device according to claim 1, characterized in that the interlayer cavity (17) has distributed therein uv lamps (18).
4. Estradiol production device according to claim 1, characterized in that said cover plate (5) is provided with a pressure gauge (51).
5. Estradiol production device according to claim 1, wherein the swirl impeller (8) comprises a blade rod (81) arranged on the rotation shaft (20), the blade rod (81) being terminated by 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. Estradiol production device according to claim 5, characterized in that the inner cylinder (3) is provided, at its bottom surface, with two layers, comprising a lower bottom plate (34) of the lower layer and a disc plate (32) of 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. Estradiol production device according to claim 1, characterized in that 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 arranged on the bottom surface of the top plate (7) through a bearing.
8. Estradiol production device according to claim 1, characterized in that the reflector of the heating tube (6) is conical.
9. A process for producing estradiol using an estradiol production facility according to any one of claims 1 to 8, characterized in that it comprises the following preparation steps:
preparation of ketal:
pumping 160-200 parts of ethylene glycol and 130-170 parts of triethyl orthoformate into a reaction kettle, adding 2-4 parts of p-toluenesulfonic acid and 130-170 parts of 1, 4-androstenedione, controlling the temperature to be 15-20 ℃, preserving heat for reaction for 2-4 hours, adding triethylamine to adjust p H-4, adding water for precipitation, 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 form a ketal;
the reaction formula is as follows:
aromatization hydrolysis reaction:
adding 1600-1700 parts of tetrahydrofuran, 45-55 parts of biphenyl, 60-70 parts of diphenylmethane and nitrogen into a reaction kettle, adjusting the temperature to 35-40 ℃, adding 7-9 parts of lithium particles, continuing to stir at 40-50 ℃ for 30 minutes, cooling to 20-25 ℃, adding 150-170 parts of the ketal, reacting at 36-40 ℃ for 2 hours, cooling to below 10 ℃, dropwise adding 450-500 parts of methanol, controlling the temperature to be lower than 35 ℃, adding 150-170 parts of hydrochloric acid, adjusting the temperature to be p H = 3-4, refluxing for 2 hours, after the reaction is finished, concentrating under reduced pressure until no solvent exists, centrifuging, washing with water, drying, putting into the drying equipment, starting the infrared heating pipe (6), irradiating for 6-10 minutes, controlling the rotating speed of the motor (19) to be 1100-1300r/min, and continuously operating for 12-18 minutes to form a hydrolysate crude product;
pumping 1000-1100 parts of ethanol into a refining kettle, adding 100-110 parts of the hydrolysate crude product and 7-9 parts of activated carbon, heating and refluxing for 30 minutes, filtering, concentrating under reduced pressure to about 3 times of volume of mother liquor, cooling to below 5 ℃, centrifuging, spin-drying, adding into the drying equipment, starting an infrared heating pipe (6), irradiating for 10-15 minutes, controlling the rotating speed of a motor (19) to be 1200-1500r/min, and continuously operating for 13-20 minutes to obtain a hydrolysate fine product;
the reaction formula is as follows:
reduction reaction and refining:
pumping 1000-1100 parts of methanol into a reaction kettle, adding the hydrolysate refined product, stirring, cooling to 0-5 ℃, adding 9-10 parts of potassium borohydride for reacting for 4-5 hours, adding glacial acetic acid for neutralizing to p H of 7, heating to 50-60 ℃, carrying out negative pressure concentration on the methanol, adding water for elutriation, carrying out centrifugal drying, putting into a drying device, starting an infrared heating pipe (6), irradiating for 4-6 minutes, controlling the rotation speed of a motor (19) to be 1200-1500r/min, and continuously operating for 8-12 minutes to obtain an estradiol crude product;
pumping 1100-1200 parts of methanol into a decoloring kettle, adding 90-100 parts of the estradiol crude product, heating to 60-65 ℃, adding 8-10 parts of activated carbon, decoloring for 1-3 hours, filtering to a crystallization kettle, reducing the pressure to 0-5 ℃ until the residual amount of mother liquor is 2 times of the weight of the product, crystallizing for 1.5-2.5 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 1200-1500r/min, and continuously operating for 12-18 minutes to obtain an estradiol refined product;
the reaction formula is as follows:
10. the process for the production of estradiol according to claim 9, characterized in that it comprises the following preparation steps:
preparation of ketal:
pumping 180 parts of ethylene glycol and 150 parts of triethyl orthoformate into a reaction kettle, adding 3 parts of p-toluenesulfonic acid and 150 parts of 1, 4-androstenedione, controlling the temperature to be 15-20 ℃, carrying out heat preservation reaction for 3 hours, adding triethylamine, adjusting p H-3.8 drops, adding 900 parts of water, carrying out elutriation, centrifuging, washing to be neutral, putting into drying equipment, starting an infrared heating pipe (6), irradiating for 10 minutes, controlling the rotating speed of a motor (19) to be 1000-1300r/min, and continuously operating for 12 minutes to form a ketal;
the aromatization hydrolysis reaction is carried out,
adding 1620 parts of tetrahydrofuran, 50 parts of biphenyl, 65 parts of diphenylmethane and nitrogen into a reaction kettle, adjusting the temperature to 35-40 ℃, adding 8.1 parts of lithium particles, continuing to stir at 40-50 ℃ for 30 minutes, cooling to 20-25 ℃, adding 162 parts of the ketal, reacting at 36-40 ℃ for 2 hours at a stirring temperature of less than or equal to 40 ℃, slowly dripping 486 parts of methanol, controlling the temperature to be less than 35 ℃, adding 162 parts of hydrochloric acid solution, adjusting p H = 3-4, heating, refluxing for 2 hours, concentrating under reduced pressure until no solvent exists after the reaction is finished, centrifuging, washing with water, 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 1100-1300r/min, and continuously operating for 15 minutes to form a hydrolysate crude product;
pumping 1050 parts of ethanol into a refining kettle, adding 105 parts of the hydrolysate crude product and 8 parts of activated carbon, heating and refluxing for 30 minutes, filtering, concentrating under reduced pressure to about 3 times of volume of mother liquor, cooling to below 5 ℃, centrifuging, spin-drying, adding into the drying equipment, starting an infrared heating pipe (6), irradiating for 12 minutes, controlling the rotating speed of a motor (19) to be 1200-1500r/min, and continuously operating for 15 minutes to obtain a hydrolysate fine product;
reduction reaction and refining:
pumping 1060 parts of methanol into a reaction kettle, adding the hydrolysate refined product, stirring, cooling to 0-5 ℃, adding 9.6 parts of potassium borohydride by times for reaction for 4-5 hours, adding glacial acetic acid for neutralization until p H is 7, heating to 50-60 ℃, concentrating the methanol under negative pressure, adding water for elutriation, centrifugally drying, putting into a drying device, starting an infrared heating pipe (6), irradiating for 5 minutes, controlling the rotation speed of a motor (19) to be 1200-1500r/min, and continuously operating for 10 minutes to obtain an estradiol crude product;
pumping 1140 parts of methanol into a decoloring kettle, adding 95 parts of the estradiol crude product, heating to 60-65 ℃, adding 9 parts of activated carbon, decoloring for 2 hours, filtering to a crystallization kettle, performing negative pressure until the residual amount of mother liquor is 2 times of the weight of the product, 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 10 minutes, controlling the rotation speed of a motor (19) to be 1200-1500r/min, and continuously operating for 15 minutes to obtain the estradiol refined product.
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