Drying equipment for medicine intermediate crystallization and drying method thereof
By setting a hot air compensation port inside the shell of the drying equipment and using a posture control mechanism, uniform drying of the crystals of the drug intermediate is achieved, solving the problem of non-uniform heat transfer in the traditional drying process, and improving the drying quality and preparation stability.
Patent Information
- Application Number
- CN202510554190.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-29
- Publication Date
- 2025-06-20
AI Technical Summary
There are problems of non-uniform heat transfer in traditional drying processes, resulting in excess of residual solvents, local overheating and drying differences, affecting the physical and chemical properties of drug intermediate crystals and the quality stability of preparations.
A drying equipment for crystallization of drug intermediates was designed, and hot air compensation ports were set up in the front, middle and rear sections of the drying box shell, and combined with the attitude control mechanism to achieve accurate control of the temperature in various parts of the shell.
Through the use of this equipment, the crystal drying of the drug intermediate can be made more uniform and sufficient, avoiding the problem of non-uniform heat transfer in the traditional drying process, and improving the drying quality and preparation stability.
Smart Images
Figure CN120176412A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of drying equipment, and particularly relates to a drying equipment for drug intermediate crystallization and a drying method thereof. Background Art
[0002] As a key link in the synthesis process of bulk drugs, the drying treatment of drug intermediate crystallization directly affects the physicochemical properties of the final product and the quality stability of the preparation. In the current pharmaceutical industry, the hot air circulation drying method (HAD) is the mainstream drying process, which mainly promotes the desorption of solvent molecules from the crystal surface through a forced convection heat transfer mechanism. However, this technology has significant technical bottlenecks in practical applications: First, it is difficult to construct a uniform temperature field distribution inside the drying chamber, and the axial and radial temperature gradients often lead to local overheating or drying blind spots; Second, the static heat transfer mode causes the "surface dry and inside wet" phenomenon of excessive drying of the surface crystals and retention of internal moisture; Third, there is a lack of a precise temperature control compensation mechanism, and thermodynamic parameters cannot be adjusted in real time according to the material accumulation form.
[0003] More notably, the non-uniform heat transfer in traditional drying processes may lead to the following quality risks: 1. Excessive residual solvents cause polymorphic transformation or chemical degradation; 2. Local overheating causes the formation of a dense layer on the crystal surface, hindering the migration of internal moisture; 3. Differences in drying degree between batches affect the subsequent mixing uniformity. Although the industry has tried to introduce alternative solutions such as microwave drying, there are generally technical pain points such as high equipment costs and poor process adaptability. Therefore, developing a dynamic drying system with intelligent temperature control compensation function to achieve precise control of the three-dimensional temperature field in the drying chamber has become the key technical breakthrough direction for improving the drying quality of drug intermediate crystallization. Summary of the Invention
[0004] The technical problem to be solved by the present invention is: to solve the problems of non-uniform heat transfer in traditional drying processes, such as excessive residual solvents causing polymorphic transformation or chemical degradation, local overheating causing the formation of a dense layer on the crystal surface, hindering the migration of internal moisture, and differences in drying degree between batches affecting the subsequent mixing uniformity. Now, a drying equipment for drug intermediate crystallization and a drying method thereof are provided.
[0005] The technical solution adopted by the present invention to solve its technical problems is: a drying equipment for drug intermediate crystallization, including a drying box with a cavity inside, and further including a control unit. The drying box is provided with a feed inlet and a drain outlet, both the feed inlet and the drain hole are communicated with the cavity, and the drying box is provided with a stirring mechanism and a circulating hot air drying mechanism. The stirring mechanism is used for stirring the drugs in the cavity and disturbing the hot air in the cavity.
[0006] The circulating hot air drying assembly includes a drying pipe, a booster pump, an air pump, a drying cylinder and a negative pressure fan. The drying pipe is arranged along the axial direction of the drying cylinder and passes through the cavity body. One end of the drying pipe is communicated with one end of the drying cylinder, the other end of the drying cylinder is communicated with the input end of the air pump, the output end of the air pump is communicated with the input end of the booster pump, the output end of the booster pump is communicated with the other end of the drying pipe. The drying pipe is provided with a plurality of interconnected hot air compensation ports in the cavity body. The plurality of hot air compensation ports are axially spaced and distributed in the front section, middle section and rear section of the drying box. Each hot air compensation port is provided with a solenoid valve, and a moisture sensor is arranged on one side of each hot air compensation port. The input end of the negative pressure fan is communicated with the cavity body of the drying box, and the output end of the negative pressure fan is communicated with one end of the drying cylinder;
[0007] It further includes an attitude control mechanism for controlling the attitude of the drying box. The control unit is respectively in signal connection with the stirring mechanism, the booster pump, the air pump, the negative pressure fan, the solenoid valve, the moisture sensor and the attitude control mechanism. Compared with the prior art, the present invention can more conveniently regulate the temperature at various parts inside the housing by arranging hot air compensation ports in the front section, middle section and rear section inside the housing, and can make the crystallization drying of the pharmaceutical intermediate inside the housing more uniform and sufficient in cooperation with the attitude control mechanism.
[0008] In some preferred embodiments, the drying pipe includes two outer ring pipes and at least two drying branch pipes. The two outer ring pipes are respectively arranged at both ends of the drying branch pipes and are connected to each other. The output end of the booster pump is communicated with one of the outer ring pipes, one end of the drying cylinder is communicated with the other outer ring pipe, a part of the drying branch pipes axially passes through and is located in the cavity body, and each drying branch pipe is provided with a hot air compensation port.
[0009] In some preferred embodiments, the attitude control mechanism includes a lower bottom plate, a first cylinder and a second cylinder. The first cylinder and the second cylinder are both fixedly installed on the upper surface of the lower bottom plate. The extending end of the first cylinder is hinged to one end of the drying box, and the extending end of the second cylinder is hinged to the other end of the drying box.
[0010] In some preferred embodiments, the drying cylinder includes an outer cylinder body, and a heating pipe and a drying plate for drying are arranged inside the outer cylinder body.
[0011] In some preferred embodiments, a plurality of heating pipes are arranged along the circumferential direction of the outer cylinder body, a plurality of drying plates are axially spaced along the outer cylinder body, the heating pipes pass through the drying plates, and a temperature and humidity sensor is arranged inside the outer cylinder body.
[0012] Preferably, in some embodiments, the stirring mechanism includes a driving motor and a spiral stirring paddle. The driving motor is fixedly installed on the drying box, and the spiral stirring paddle is arranged in the cavity body and is in transmission connection with the driving motor.
[0013] Preferably, in some embodiments, a pressure sensor is arranged between the other end of the booster pump and the drying pipe, and a one-way valve is arranged between one end of the drying pipe and the drying cylinder.
[0014] A drying method using the drying equipment for drug intermediate crystallization as described above, and the specific operation steps are as follows:
[0015] When drying the drug intermediate crystallization, hot air is pumped from the air outlet of the air pump in the a direction to the other end of the drying pipe and transported to one end;
[0016] The user sets the time capable of completing the drying process as t. When controlling the amount of drug intermediate crystallization placed in the drying box each time and the rotation speed value of the stirring mechanism to be stable, after the drying process is completed, a moisture sensor is used to detect the dryness of the dried drug intermediate crystallization. The detected data is transmitted to the control unit. The control unit sets the minimum qualified dryness value after the drying process as p, sets the maximum qualified dryness value after the drying process as m, and sets the dryness detected by the moisture sensor after the drying process at each place as w;
[0017] When the drying time of the drug intermediate crystallization by the drying pipe reaches t, the moisture sensors located in the front section, middle section, and rear section inside the drying box will detect the drying index w of the drug intermediate crystallization at each place inside it, and the moisture sensors will send the detected data to the control unit. The control unit will compare the received drying indices w at each place with p and m respectively:
[0018] Compare the monitoring data of the front section, middle section, and rear section of the drying box with the preset values in the control unit respectively. If the drying indices w in the front section, middle section, and rear section of the drying box are all within the range of p≤w≤m, the dryness of the drug intermediate crystallization in this section reaches the qualified standard, and it can be taken out after drying;
[0019] If there is any section in the front section, middle section, and rear section of the drying box where w < p, continue to make adjustments.
[0020] Preferably, in some embodiments, within the time t, when only and only one section among the front section, middle section, and rear section of the drying box has w < p, it is divided into the following situations:
[0021] When the drying index w of the front or rear section of the drying oven is less than p, and the drying indices of the other two sections are within the range of p ≤ w ≤ m, in this case, regardless of whether the drying index w of the front or rear section of the drying oven is less than p, the drying index w of the middle section of the drying oven is always within the range of p ≤ w ≤ m. The control unit controls the drying index w to be less than p and controls the attitude control mechanism to place the drying oven in an inclined state, so as to move the crystallization of the pharmaceutical intermediate at this place to the other two sections where the drying index w is within the range of p ≤ w ≤ m for mixing. The crystallization of the pharmaceutical intermediate at the place where the drying index w in the drying oven is less than p is fully mixed with the qualified crystallization of the pharmaceutical intermediate at the other two places, and drying continues until the drying index w of the mixed crystallization in the front and middle sections or the middle and rear sections inside the drying oven is dried to within the range of p ≤ w ≤ m;
[0022] When the drying index w of the middle section of the drying oven is less than p, and the drying indices w of the front and rear sections are within the range of p ≤ w ≤ m, the control unit controls the attitude control mechanism to fully mix the crystallization of the pharmaceutical intermediate with a qualified drying index w in the front and rear sections of the drying oven with the crystallization of the pharmaceutical intermediate at the place where the drying index w of the middle section is less than p, and drying continues until the drying indices w of the front, middle, and rear sections of the drying oven are all dried to within the range of p ≤ w ≤ m;
[0023] Within time t, if there are two sections among the front, middle, and rear sections of the drying oven with w < p, then it is divided into the following situations:
[0024] When the drying indices w of two sections among the front and middle sections, front and rear sections, or middle and rear sections of the drying oven are less than p, the control unit controls the attitude control mechanism to fully mix the crystallization of the pharmaceutical intermediate at the place where the drying index w is less than p with the crystallization of the pharmaceutical intermediate at the place where the drying index w is within the range of p ≤ w ≤ m, and the control unit controls the hot air compensation ports corresponding to the two places where the drying index w is less than p to open, and uses the hot air compensation ports to perform temperature compensation on the crystallization of the pharmaceutical intermediate at the place where the drying index w is less than p. Drying continues. After drying for time t, if the drying indices w of the front, middle, and rear sections of the drying oven are all within the range of p ≤ w ≤ m, it indicates that the drying process is completed.
[0025] Preferably, in some embodiments, after drying for t hours, if the drying index w at the front, middle, and rear sections of the drying oven still has the situation where w < p, it is necessary to check the airtightness inside the drying oven. Mix the drug intermediate crystals at the location where the drying index w < p with the drug intermediate crystals at the location where the drying index w is within the range of p ≤ w ≤ m, and the control unit controls the hot air compensation port at the location where the drying index w < p to open. Without changing other variables, let it stand for a period of time, and then measure the temperature inside the drying oven using a thermometer. If, after standing for a period of time, the temperature reduction index inside the drying oven is greater than the temperature reduction index inside a drying oven with good airtightness under the same time period, it indicates that there is an air leakage in the drying oven, which affects the drying efficiency. At this time, increase the drying time t until the drying index w at the front, middle, and rear sections of the drying oven is dried to within the range of p ≤ w ≤ m. After drying is completed, repair or replace the air leakage location of the drying oven.
[0026] The beneficial effects of the present invention are as follows: When the drying equipment and drying method for drug intermediate crystals of the present invention are in use, by setting hot air compensation ports at the front, middle, and rear sections inside the housing, and cooperating with the attitude control mechanism, it is more convenient to control the temperature at various locations inside the housing, so that the drug intermediate crystals inside the housing can be dried more evenly and fully, avoiding the problems of non-uniform heat transfer in the traditional drying process, such as excessive residual solvents causing crystal form transformation or chemical degradation, local overheating resulting in the formation of a dense layer on the crystal surface, hindering the migration of internal moisture, and the difference in drying degree between batches affecting the subsequent mixing uniformity. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] The present invention will be further described below with reference to the drawings and embodiments.
[0028] Figure 1 is the three-dimensional structure diagram of the present invention;
[0029] Figure 2 is the installation structure diagram between the drying oven 1 and the circulating hot air drying component in the present invention;
[0030] Figure 3 is Figure 2 the partial enlarged view of A in
[0031] Figure 4 is Figure 2 the partial enlarged view of B in
[0032] Figure 5 is the structure diagram of the drying cylinder in the present invention;
[0033] Figure 6 is Figure 5 the partial enlarged view of C in
[0034] Figure 7 This is a schematic structural view of the present invention during drying.
[0035] In the figure: 1. drying oven, 101. cavity body, 102. feed inlet, 103. drain outlet, 2. drying pipe, 3. booster pump, 4. air pump, 5. drying cylinder, 6. negative pressure fan, 7. hot air compensation port, 8. moisture sensor, 9. outer ring pipe, 10. drying branch pipe, 11. lower bottom plate, 12. first cylinder, 13. second cylinder, 14. outer cylinder body, 15. heating pipe, 16. drying plate, 17. temperature and humidity sensor, 18. drive motor, 19. spiral stirring paddle, 20. pressure sensor, 21. one-way valve, 22. control unit. Specific embodiments
[0036] The present invention will be further described in detail below in conjunction with embodiments:
[0037] The present invention is not limited to the following specific embodiments. Those of ordinary skill in the art can implement the present invention in other various specific embodiments according to the content disclosed in the present invention, or any simple changes or modifications made using the design structure and concept of the present invention fall within the protection scope of the present invention. It should be noted that, without conflict, the embodiments in the present invention and the features in the embodiments can be combined with each other.
[0038] In the description of the present invention, it should be understood that the orientation or positional relationship indicated by the terms "center", "longitudinal", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus cannot be understood as a limitation to the present invention. In addition, the terms "first", "second", etc. are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, the features defined with "first", "second", etc. may explicitly or implicitly include one or more of such features. In the description of the present invention, unless otherwise specified, the meaning of "a plurality" is two or more.
[0039] In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, the terms "installation", "connection", and "coupling" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, and it can be the communication inside two components. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0040] Embodiment 1
[0041] As Figure 1-7 shown, a drying device for crystallizing a pharmaceutical intermediate includes a drying box 1, a control unit 22, and an attitude control mechanism. The drying box 1 has a cavity 101 inside. The drying box 1 is provided with a feed inlet 102 and a drain outlet 103. The feed inlet 102 faces upward and is located above one end of the drying box 1, and the drain outlet 103 faces downward and is located below the other end of the drying box 1. The feed inlet 102 and the drain hole are both communicated with the cavity 101. The drying box 1 is provided with a stirring mechanism and a circulating hot air drying mechanism. The stirring mechanism is used for stirring the medicine in the cavity 101 and disturbing the hot air in the cavity 101.
[0042] The circulating hot air drying assembly includes a drying pipe 2, a booster pump 3, an air pump 4, a drying cylinder 5, and a negative pressure fan 6. The drying pipe 2 is arranged along the axial direction of the drying cylinder 5 and passes through the cavity 101. One end of the drying pipe 2 is communicated with one end of the drying cylinder 5. The other end of the drying cylinder 5 is communicated with the input end of the air pump 4. The output end of the air pump 4 is communicated with the input end of the booster pump 3. The output end of the booster pump 3 is communicated with the other end of the drying pipe 2. The drying pipe 2 is provided with a plurality of mutually communicated hot air compensation ports 7 in the cavity 101. The plurality of hot air compensation ports 7 are axially spaced and distributed in the front section, middle section, and rear section of the drying box 1. Each hot air compensation port 7 is provided with a solenoid valve, and a moisture sensor 8 is arranged on one side of each hot air compensation port 7. The input end of the negative pressure fan 6 is communicated with the cavity 101 of the drying box 1, and the output end of the negative pressure fan 6 is communicated with one end of the drying cylinder 5.
[0043] The attitude control mechanism is used to control the attitude of the drying box 1. The control unit 22 is respectively signal-connected to the stirring mechanism, the booster pump 3, the air pump 4, the negative pressure fan 6, the solenoid valve, the moisture sensor 8, and the attitude control mechanism. The drying box 1 is controlled to be in a horizontal state or an inclined state by controlling the expansion and contraction of the extending ends of the first cylinder 12 and the second cylinder 13.
[0044] The drying tube 2 includes two outer ring tubes 9 and three drying branch tubes 10. The outer ring tube 9 is a ring structure. The two outer ring tubes 9 are respectively arranged at the two ends of the three drying branch tubes 10 and are connected to each other. The three drying branch tubes 10 are arranged parallel to each other. The output end of the booster pump 3 is connected to an outer ring tube 9 on the right, and one end of the drying cylinder 5 is connected to another outer ring tube 9. A part of the drying branch tube 10 passes through the drying box 1 axially and is located in the cavity 101. Each drying branch tube 10 is provided with a hot air compensation port 7.
[0045] The posture control mechanism includes a lower base plate 11, a first cylinder 12 and a second cylinder 13. The first cylinder 12 and the second cylinder 13 are both fixedly mounted on the upper surface of the lower base plate 11. The protruding end of the first cylinder 12 is hinged at the left end of the drying box 1, and the protruding end of the second cylinder 13 is hinged at the right end of the drying box 1. In order to ensure that the drying box 1 is smooth during posture adjustment, a connecting hose is installed between the outer ring tube 9 on one side of the drying box 1 and the booster pump 3, a connecting hose is also installed between the outer ring tube 9 on the other side of the drying box 1 and the one-way valve 21, and a connecting hose is also installed between the output end of the negative pressure fan 6 and the drying cylinder 5.
[0046] The drying cylinder 5 includes an outer cylinder body 14, in which a heating tube 15 and a drying plate 16 for drying are arranged. Several heating tubes 15 are arranged along the circumferential direction of the outer cylinder body 14, and several drying plates 16 are arranged at intervals along the axial direction of the outer cylinder body 14. The heating tube 15 passes through the drying plate 16. A temperature and humidity sensor 17 is arranged in the outer cylinder body 14. When the temperature and humidity sensor 17 in the drying cylinder 5 detects that the internal air temperature is lower than the set value in the control unit 22, the temperature and humidity sensor 17 sends the monitoring signal to the control unit 22 by wireless transmission. The control unit 22 controls the electric heating tube 15 to start, so as to heat the internal temperature of the drying cylinder 5 until the internal temperature of the drying cylinder 5 is heated to the set value of the control unit 22. The drying plate 16 and the electric heating tube 15 are both used to dry and heat the air recovered from the inside of the drying box 1 so as to continue to circulate it.
[0047] The stirring mechanism includes a driving motor 18 and a spiral stirring paddle 19. The driving motor 18 is fixedly mounted on the drying box 1. The spiral stirring paddle 19 is arranged in the cavity body 101 and is transmission-connected to the driving motor 18. A cavity is opened inside the spiral stirring paddle, and the cavity is used to fill a heating medium, which can be hot oil.
[0048] A pressure sensor 20 is provided between the other end of the booster pump 3 and the other end of the drying pipe 2. A one-way valve 21 is provided between one end of the drying pipe 2 and the drying cylinder 5. In this embodiment, the moisture sensor 8 can be an infrared moisture sensor 8, which mainly utilizes the infrared light absorption characteristics to detect the moisture content by measuring the absorption amount of the object to the infrared light of a specific wavelength. This is the prior art and will not be elaborated here. The moisture sensor 8 is mainly used to monitor the drying degree of the drug intermediate crystal.
[0049] The negative pressure fan 6 is used to absorb the water vapor generated when the hot air dries the drug intermediate crystal in the drying oven 1 and convey it to the drying cylinder 5. When the hot air enters from the drying pipe 2 on the right side of the drying oven 1 and dries the drug intermediate crystal in the drying oven 1, a certain amount of water vapor will be generated inside the drying oven 1. Start the negative pressure fan 6, and the negative pressure fan 6 will convey the water vapor and negative pressure inside the drying oven 1 to the drying cylinder 5. The one-way valve 21 is used to prevent the water vapor from flowing back to the drying pipe 2. Then, by using the negative pressure generated by the air pump 4, the absorbed water vapor is dried and heated along the gas flow direction through the drying cylinder 5, and finally conveyed by the air pump 4 again for repeated use.
[0050] It should be further noted that in order to keep the drying efficiency of the drug intermediate crystal inside the drying oven 1 relatively stable, a standard pressure value inside the pipeline is integrally set in the control unit 22. When the negative pressure fan 6 starts to work, the pressure sensor 20 will monitor the air pressure inside the drying pipe 2. When the air pressure inside the drying pipe 2 is lower than the standard pressure value set in the control unit 22, start the booster pump 3. The booster pump 3 increases the pressure inside the pipeline by sucking, compressing and discharging gas or liquid, so that the pressure value inside the pipeline reaches the set standard pressure value, preventing the pressure inside the pipeline from decreasing and the gas flow rate from decreasing, thereby affecting the drying efficiency of the drug intermediate crystal.
[0051] Embodiment 2
[0052] Embodiment 2 is a drying method using the drying equipment in Embodiment 1. Specifically: A drying method using a drying equipment for drug intermediate crystal as described above, and the specific operation steps are as follows:
[0053] When drying the drug intermediate crystal, the hot air is pumped into the drying pipe 2 in the a direction through the air pump 4, and then the dried hot air is pumped into the drying cylinder 5 in the b direction. When the dried hot air enters the drying pipe 2, since both ends of the plurality of drying branch pipes 10 are respectively communicated with the outer ring pipes 9 on both sides, at this time, the hot air inside the outer ring pipe 9 continues to be conveyed to the drying branch pipe 10 on the other side in the c direction, and the heat carried by the hot air inside the drying branch pipe 10 is used to dry the drug intermediate crystal;
[0054] The user can set the time for completing the drying process to t. When the amount of the drug intermediate crystals placed in the drying oven 1 each time and the rotational speed value of the stirring mechanism remain stable, after the drying process is completed, the moisture sensor 8 is used to detect the dryness of the dried drug intermediate crystals, and the detected data is transmitted to the control unit 22. The control unit 22 sets the minimum qualified dryness value after the drying process is completed to p, the maximum qualified dryness value after the drying process is completed to m, and sets the dryness detected by the moisture sensor 8 after the drying process at each location to w;
[0055] When the drying time of the drug intermediate crystals by the drying tube 2 reaches t, the moisture sensors 8 located in the front section, middle section, and rear section inside the drying oven 1 will detect the drying index w of the drug intermediate crystals at each location inside it. The moisture sensors 8 will send the detected data to the control unit 22, and the control unit 22 will compare the received drying indices w at each location with p and m respectively:
[0056] The monitoring data of the front section, middle section, and rear section of the drying oven 1 are respectively compared with the preset values in the control unit 22. If the drying indices w in the front section, middle section, and rear section of the drying oven 1 are all within the range of p ≤ w ≤ m, then the dryness of the drug intermediate crystals in this section reaches the qualified standard, and they can be taken out after drying;
[0057] If in any section of the front section, middle section, and rear section of the drying oven 1, there is a situation where w < p, then continue to make adjustments.
[0058] Within the time t, if only and only one section in the front section, middle section, and rear section of the drying oven 1 has w < p, then it is divided into the following situations:
[0059] When the drying index w of one section in the front section or rear section of the drying oven 1 is less than p, and the drying indices of the other two sections are within the range of p ≤ w ≤ m. In this case, regardless of whether the drying index w of the front section or rear section of the drying oven 1 is less than p, the drying index w of the middle section of the drying oven 1 is within the range of p ≤ w ≤ m. The control unit 22 controls the drying index w < p, and controls the attitude control mechanism to place the drying oven 1 in an inclined state, and moves the drug intermediate crystals at this location to the other two sections where the drying indices are within the range of p ≤ w ≤ m for mixing. The drug intermediate crystals with a drying index w < p inside the drying oven 1 are fully mixed with the qualified drug intermediate crystals at the other two locations, and continue to be dried until the drying index w of the mixed crystals in the front section and middle section inside the drying oven 1 or the mixed crystals in the middle section and rear section inside the drying oven 1 is dried to within the range of p ≤ w ≤ m;
[0060] When the drying index w in the middle section of the drying oven 1 is less than p, and the drying indices w in the front and rear sections are within the range of p ≤ w ≤ m, the control unit 22 controls the attitude control mechanism to fully mix the drug intermediate crystals with qualified drying index w in the front and rear sections of the drying oven 1 with the drug intermediate crystals at the middle section where the drying index w < p, and continue drying until the drying indices w in the front, middle, and rear sections of the drying oven 1 are all dried within the range of p ≤ w ≤ m;
[0061] Within the time t, if there are two sections among the front, middle, and rear sections of the drying oven 1 with w < p, then it is divided into the following situations:
[0062] When the drying indices w of two sections among the front and middle sections, front and rear sections, or middle and rear sections of the drying oven 1 are less than p, the control unit 22 controls the attitude control mechanism to fully mix the drug intermediate crystals at the places where the drying index w < p with the drug intermediate crystals at the places where the drying index w is within the range of p ≤ w ≤ m, and the control unit 22 controls the hot air compensation ports 7 corresponding to the two places where the drying index w < p to open, and uses the hot air compensation ports 7 to perform temperature compensation on the drug intermediate crystals at the places where the drying index w < p, and continue drying. After drying for the time t, if the drying indices w of the three places of the front, middle, and rear sections of the drying oven 1 are all within the range of p ≤ w ≤ m, it indicates that the drying process is completed.
[0063] After drying for the time t, if there is still a situation where w < p in the drying indices w of the three places of the front, middle, and rear sections of the drying oven 1, it is necessary to check the airtightness inside the drying oven 1, fully mix the drug intermediate crystals at the places where the drying index w < p with the drug intermediate crystals at the places where the drying index w is within the range of p ≤ w ≤ m, and the control unit 22 controls the hot air compensation ports 7 at the places where the drying index w < p to open. Without changing other variables, let it stand for a period of time, and then measure the temperature inside the drying oven 1 by using a thermometer. If after standing for a period of time, the temperature reduction index inside the drying oven 1 is greater than the temperature reduction index inside the drying oven 1 with good airtightness under the same time, it indicates that there is an air leakage situation in the drying oven 1 that affects the drying efficiency. At this time, increase the drying time t until the drying indices w of the three places of the front, middle, and rear sections of the drying oven 1 are dried within the range of p ≤ w ≤ m. After drying is completed, repair or replace the air leakage part of the drying oven 1.
[0064] Based on the ideal embodiments of the present invention as inspiration, through the above description, relevant staff can completely make various changes and modifications without departing from the technical idea of this invention. The technical scope of this invention is not limited to the content in the specification, and its technical scope must be determined according to the scope of the claims.
Claims
1. A drying device for crystallization of a pharmaceutical intermediate, comprising a drying box having a cavity inside, characterized in that: It also includes a control unit, the drying box is provided with a feed inlet and a drain hole, the feed inlet and the drain hole are both connected to the cavity, the drying box is provided with a stirring mechanism and a circulating hot air drying mechanism, the stirring mechanism is used to stir the medicine in the cavity and disturb the hot air in the cavity; The circulating hot air drying component includes a drying tube, a booster pump, an air pump, a drying cylinder and a negative pressure fan. The drying tube is axially arranged along the drying cylinder and passes through a hollow cavity. One end of the drying tube is connected to one end of the drying cylinder, and the other end of the drying cylinder is connected to an input end of the air pump. The output end of the air pump is connected to the input end of the booster pump, and the output end of the booster pump is connected to the other end of the drying tube. The drying tube is provided with a plurality of interconnected hot air compensation ports in the hollow cavity. The plurality of hot air compensation ports are axially spaced and distributed at intervals in the front section, middle section and rear section of the drying box. A solenoid valve is provided on each of the hot air compensation ports, and a moisture sensor is provided on one side of each of the hot air compensation ports. The input end of the negative pressure fan is connected to the hollow cavity of the drying box, and the output end of the negative pressure fan is connected to one end of the drying cylinder. It also includes a posture control mechanism, which is used to control the posture of the drying box. The control unit is respectively connected to the stirring mechanism, the booster pump, the air pump, the negative pressure fan, the solenoid valve, the moisture sensor and the posture control mechanism by signal.
2. A drying device for crystallization of a pharmaceutical intermediate according to claim 1, characterized in that: The drying tube includes two outer ring tubes and at least two drying branch tubes, the two outer ring tubes are respectively arranged at the two ends of the drying branch tubes and are connected to each other, the output end of the booster pump is connected to one of the outer ring tubes, and one end of the drying cylinder is connected to the other outer ring tube. A part of the drying branch tube passes through the drying box axially and is located in the cavity, and each of the drying branch tubes is provided with a hot air compensation port.
3. A drying device for crystallization of a pharmaceutical intermediate according to claim 1, characterized in that: The posture control mechanism includes a lower base plate, a first cylinder and a second cylinder, wherein the first cylinder and the second cylinder are both fixedly mounted on the upper surface of the lower base plate, the protruding end of the first cylinder is hinged to one end of the drying box, and the protruding end of the second cylinder is hinged to the other end of the drying box.
4. A drying device for crystallization of a pharmaceutical intermediate according to claim 1, characterized in that: The drying cylinder comprises an outer cylinder body, in which a heating tube and a drying plate for drying are arranged.
5. A drying device for crystallization of a pharmaceutical intermediate according to claim 4, characterized in that: The heating tubes are arranged in a plurality along the circumferential direction of the outer cylinder, the drying plates are arranged in a plurality along the axial direction of the outer cylinder at intervals, the heating tubes pass through the drying plates, and a temperature and humidity sensor is arranged in the outer cylinder.
6. A drying device for crystallization of a pharmaceutical intermediate according to claim 1, characterized in that: The stirring mechanism comprises a driving motor and a spiral stirring paddle. The driving motor is fixedly mounted on the drying box, and the spiral stirring paddle is arranged in the cavity and is drivingly connected to the driving motor.
7. A drying device for crystallization of a pharmaceutical intermediate according to claim 1, characterized in that: A pressure sensor is arranged between the booster pump and the other end of the drying pipe, and a one-way valve is arranged between one end of the drying pipe and the drying cylinder.
8. A drying method using a drying device for crystallization of a pharmaceutical intermediate according to any one of claims 1 to 7, characterized in that: The specific steps are as follows: When drying the crystals of the pharmaceutical intermediate, the hot air is pumped in direction a through the air outlet of the air pump to the other end of the drying tube and transported to one end; The user sets the time to complete the drying process as t, controls the amount of drug intermediate crystals placed in the drying box at a time, and the speed value of the stirring mechanism remains stable. After the drying process is completed, the moisture sensor is used to detect the dryness of the drug intermediate crystals after drying. The detected data is transmitted to the control unit. The control unit sets the minimum value of the qualified dryness after the drying process is completed as p, the maximum value of the qualified dryness after the drying process is completed as m, and the dryness detected by the moisture sensor at each location after the drying process is completed as w; When the drying time of the drug intermediate crystallization in the drying tube reaches t, the moisture sensors located in the front, middle and rear sections of the drying oven will detect the drying index w of the drug intermediate crystallization at various locations inside. The moisture sensors will send the detected data to the control unit, and the control unit will compare the received drying index w with p and m respectively: The monitoring data of the front section, middle section and rear section of the drying oven are respectively compared with the preset values in the control unit. If the drying index w in the front section, middle section and rear section of the drying oven is within the range of p≤w≤m, the dryness of the drug intermediate crystals in this section meets the qualified standard and can be taken out after drying. If w<p exists in any section among the front section, middle section and rear section of the drying box, continue to make adjustments.
9. The drying method according to claim 8, characterized in that: Within the time t, when there is only one section w<p in the front section, middle section and back section of the drying oven, it can be divided into the following situations: When the drying index of one section of the front section or the rear section of the drying oven is w<p, and the drying indexes of the other two sections are within the range of p≤w≤m, in this case, no matter the drying index of the front section or the rear section of the drying oven is w<p, the drying index w of the middle section of the drying oven is within the range of p≤w≤m, the control unit controls the drying index w<p, and controls the posture control mechanism to place the drying oven in an inclined state, and moves the drug intermediate crystals at this location to the other two sections where the drying index is within the range of p≤w≤m for mixing, and the drug intermediate crystals at the drying index w<p inside the drying oven are fully mixed with the qualified drug intermediate crystals at the other two locations, and continue to dry until the drying index w of the mixed crystals in the front section and the middle section inside the drying oven or the mixed crystals in the middle section and the rear section inside the drying oven is dried to the range of p≤w≤m; When the drying index w of the middle section of the drying oven is less than p, and the drying index w of the front section and the rear section is within the range of p≤w≤m, the control unit controls the posture control mechanism to fully mix the drug intermediate crystals with the qualified drying index w in the front section and the rear section of the drying oven with the drug intermediate crystals with the drying index w<p in the middle section, and continue to dry until the drying index w of the front section, the middle section, and the rear section of the drying oven are all dried to the range of p≤w≤m; Within the time t, if there are two sections in the front section, middle section, and rear section of the drying oven where w < p, it can be divided into the following situations: When the drying index w of two sections among the front section and the middle section, the front section and the rear section, or the middle section and the rear section of the drying oven is less than p, the control unit controls the posture control mechanism to fully mix the drug intermediate crystals at the drying index w<p with the drug intermediate crystals at the drying index w within the range of p≤w≤m, and the control unit controls the hot air compensation ports corresponding to the two places with the drying index w<p to open, and uses the hot air compensation ports to perform temperature compensation for the drug intermediate crystals at the drying index w<p, and continues to dry. After drying for time t, if the drying indexes w at the front section, the middle section, and the rear section of the drying oven are all within the range of p≤w≤m, it means that the drying process is completed.
10. The drying method according to claim 9, characterized in that: After drying for t time, if the drying index w at the front section, middle section and rear section of the drying box still shows w<p, the air tightness inside the drying box needs to be checked, and the drug intermediate crystals at the drying index w<p are fully mixed with the drug intermediate crystals at the drying index w within the range of p≤w≤m, and the control unit controls the hot air compensation port 7 at the drying index w<p to open. While ensuring that other variables remain unchanged, let it stand for a period of time, and then measure the temperature inside the drying box by using a thermometer. If, after standing for a period of time, the temperature reduction index inside the drying box is greater than the temperature reduction index inside the drying box with intact sealing at the same time, it means that there is leakage in the drying box, which affects the drying time. At this time, increase the drying time t until the drying index w at the front section, middle section and rear section of the drying box is dried to within the range of p≤w≤m. After drying, the leaking part of the drying box is repaired or replaced.