A raw material drying storage device and method for producing pharmaceutical intermediates

Abstract

The invention discloses a raw material drying and storage device and method for producing pharmaceutical intermediates, comprising a box body and a lower hopper, wherein the box body is connected with the lower hopper, and a discharge pipe is connected at the bottom of the lower hopper, and a discharge electric control valve is arranged at the position of the discharge pipe. When the pharmaceutical intermediate raw material in the box body is taken out, a circulation pipe introduces external air into the box body, and after the raw material is taken out, the horizontal line of the pharmaceutical intermediate raw material in the box body will drop. After the raw material taking-out operation is completed, a hot air supply mechanism is started, a heat pipe and an air outlet pipe are connected, and dry hot air is transported into the box body and the residual air in the box body is continuously discharged. At the same time, after a distance sensor module detects that the upper surface position of the raw material has dropped, a heating resistor within a certain depth range of the upper surface of the raw material and below is controlled to work, and moist air that may exist in the gap between the raw materials is discharged, so as to avoid the occurrence of problems such as moisture and agglomeration caused by excessive contact time between the upper raw material and the outside air after the outside air enters.

Description

Technical Field

[0001] The invention relates to the technical field of pharmaceutical intermediate storage, in particular to a raw material drying and storage device for pharmaceutical intermediate production. Background Art

[0002] Pharmaceutical intermediates are actually some chemical raw materials or chemical products used in the process of drug synthesis. This kind of chemical product does not require a drug production license and can be produced in an ordinary chemical plant. As long as it reaches a certain level, it can be used for drug synthesis. When processing pharmaceutical intermediates, in order to extend the use cycle of pharmaceutical intermediates, people will use dry storage devices to dry the pharmaceutical intermediates.

[0003] In the existing processing methods, since pharmaceutical intermediate raw materials are usually in powder form, one method is to pour the pharmaceutical intermediate raw materials directly into a storage tank, and then insert a number of heating rods into the tank to ensure that the pharmaceutical intermediate raw materials will not clump or get damp during storage.

[0004] In actual production, materials are taken from storage tanks at irregular intervals. Since storage tanks are generally in a vacuum state, air needs to be transported into the storage tanks when taking materials to facilitate the unloading of pharmaceutical intermediate raw materials. However, after the outside air enters the storage tank, the air will come into contact with the pharmaceutical intermediate raw materials at the top, causing the pharmaceutical intermediate raw materials to be contaminated. The longer the contact time with air, the more serious the contamination of the pharmaceutical intermediate raw materials at the top.

[0005] The existing treatment methods are to reduce the material collection time when discharging the pharmaceutical intermediates to reduce the contact time between the outside air and the pharmaceutical intermediate raw materials, or to convey dry hot air into the box at the same time when discharging, and stop conveying dry hot air until the discharging is completed. However, when this method is used, if the discharging time is long, dry hot air needs to be conveyed into the box all the time, which has a high industrial cost.

[0006] In the face of the above situation, how to effectively solve the problem of the upper layer of raw materials of pharmaceutical intermediates being contaminated by contact with the air when taking the raw materials has become a difficult problem. Summary of the invention

[0007] In order to solve the above technical problems, the present invention provides a raw material drying and storage device for the production of pharmaceutical intermediates, which realizes that after taking out a number of pharmaceutical intermediate raw materials, the pharmaceutical intermediate raw materials at the top that are in contact with the air can be heated in a targeted manner through the cooperation of a distance sensing module and a heating resistor, thereby preventing the pharmaceutical intermediate raw materials at the top from being in contact with the outside air for too long, causing raw material contamination.

[0008] To achieve the above-mentioned purpose, the present invention provides the following technical solutions: a raw material drying and storage device for the production of pharmaceutical intermediates, comprising a box body and a lower hopper, the box body is connected to the lower hopper, the bottom of the lower hopper is connected to a discharge pipe, a discharge electric control valve is arranged at the position of the discharge pipe, raw materials are stored in the box body to form a raw material area, and a gas area is formed on the upper side of the raw material area in the inner cavity of the box body.

[0009] A sealing cover is arranged on the top of the box body, a distance sensor module is fixedly arranged on the bottom side of the sealing cover, a plurality of heating rods are fixedly arranged on the bottom side of the sealing cover, and a plurality of heating resistors are arranged on the surface of the heating rods at equal intervals from top to bottom.

[0010] A heat pipe is connected to one side of the upper gas area of ​​the box, an outlet pipe is connected to the other side of the upper gas area of ​​the box, a flow pipe is connected to the surface of the heat pipe, a dry hot air supply mechanism is arranged upstream of the heat pipe, the heat pipe is arranged with a first electrically controlled valve for controlling the hot air flow interruption, the flow pipe is arranged with a second electrically controlled valve, and the outlet pipe is arranged with a third electrically controlled valve.

[0011] The inner wall of the box is provided with a humidity sensor module located in the gas area.

[0012] As a preferred technical solution of the present invention, the resistance values ​​of the multiple heating resistors on the heating rod are the same.

[0013] As a preferred technical solution of the present invention, the resistance values ​​of the multiple heating resistors on the heating rod increase from top to bottom.

[0014] As a preferred technical solution of the present invention, based on the direction of hot air flow injected into the box by the heat pipe, the position where the circulation pipe is connected to the heat pipe is located on the downstream side of the first electric control valve.

[0015] As a preferred technical solution of the present invention, the bottom of the box is connected to the top of the lower hopper, and the lower side end of the heating rod extends to the top area of ​​the lower hopper.

[0016] As a preferred technical solution of the present invention, among the heating resistors distributed on the heating rod, the horizontal position of the highest heating resistor is lower than the horizontal positions of the heat flux pipe and the air outlet pipe.

[0017] The present invention provides a method for using a raw material drying and storage device for producing a pharmaceutical intermediate, comprising the following steps:

[0018] S1. Open the sealing cover and pour the pharmaceutical intermediate raw materials to be stored into the box. A number of heating rods are arranged inside the sealing cover. The heating rods are powered on to heat and dry the pharmaceutical intermediate raw materials placed inside the box.

[0019] S2. During the process of storing pharmaceutical intermediate raw materials, when a part of the pharmaceutical intermediate raw materials needs to be taken out from the box, the discharge electric control valve and the second electric control valve are opened, and the outside air flows into the box from the circulation pipe, and the discharge pipe discharges downward, and the pharmaceutical intermediate raw materials stored in the box flow out from the discharge pipe.

[0020] S3. After the pharmaceutical intermediate raw materials are taken out, the discharge electric control valve and the second electric control valve are closed, so as to stop the air intake of the circulation pipe and the discharge of the discharge pipe. The dry hot air supply mechanism is started, the first electric control valve on the heat pipe is opened, and the third electric control valve on the outlet pipe is opened. The dry hot air flow enters the interior of the box from the heat pipe to discharge the residual air in the gas area of ​​the box.

[0021] S4. Assume that the vertical distances between the heating resistors of the heating rod and the distance sensor module are {L1, L2, L3, ..., L n}.

[0022] When the distance sensor module detects that the distance between the upper surface of the pharmaceutical intermediate material after the discharge operation is completed is Ls, it is determined that Ls is the distance between {L1, L2, L3, ..., L n}Relationship:

[0023] Let L s ∈[L x-1 , L x ], then the control system drives L x-1 ~L x+m Heating is performed by a heating resistor within the range.

[0024] Among them, L x-1 ∈{L1, L2, L3, ..., L n}, L x ∈{L1, L2, L3, ..., L n}, L x+m ∈{L1, L2, L3, ..., L n}.

[0025] Among them, L x+m m∝The distance sensor module detects the distance L in real time s , distance L s The larger it is, the larger the volume of the gas area in the box. When the circulation pipe is opened to let the outside air in, the more outside air enters, and the greater the impact on the moisture of the upper surface of the pharmaceutical intermediate raw materials may be.

[0026] By heating the raw materials within a certain depth range on the upper surface of the pharmaceutical intermediate raw materials, the gas in the gaps between the raw materials within a certain depth range on the upper surface of the pharmaceutical intermediate raw materials can expand and escape upward, directly discharging the moisture source to a certain depth on the upper surface of the raw materials. The reason why the middle and lower layers of raw materials are not heated is that the air entering the box will basically contact the surface area of ​​the raw materials, and the raw materials in the middle and lower layers are difficult to directly contact the air in the upper part of the box. In addition, the raw materials in the middle and lower layers are squeezed by the gravity of the upper raw materials, and the gaps between the raw materials are relatively small. The gaps between the raw materials within a certain depth range on the upper surface of the raw materials are large, and it is easy to hide the outside air.

[0027] S5. Dry hot air flows into the box from the heat pipe. The humidity sensor module in the box monitors the gas humidity parameters in real time. When the gas humidity parameter in the box is lower than the minimum humidity reference value ψ preset by the system min When the time period that the temperature remains below the reference value is greater than the reference time period t preset by the system, the dry hot air supply mechanism stops, the first electrically controlled valve of the heat pipe is closed, and the third electrically controlled valve of the air outlet pipe is closed.

[0028] The present invention provides a raw material drying and storage device for the production of pharmaceutical intermediates, which has the following beneficial effects:

[0029] When the pharmaceutical intermediate raw material in the box is taken out, the external air is introduced into the box through the circulation pipe. After the pharmaceutical intermediate raw material is taken out, the horizontal line of the pharmaceutical intermediate raw material in the box will drop. After the operation of taking out the pharmaceutical intermediate raw material is completed, the hot air supply mechanism is started, the heat pipe and the air outlet pipe are connected, and the dry hot air is transported into the box and the residual air in the box is continuously discharged. At the same time, after the distance sensor module detects that the position of the upper surface of the raw material has dropped, the heating resistor within a certain depth range of the upper surface of the raw material and below is controlled to work, and the gas remaining on the upper surface of the raw material and within a certain depth range below is thermally expanded, and the humid air that may exist in the gap between the raw materials is discharged, so as to avoid the occurrence of problems such as moisture and agglomeration caused by the upper raw material being in contact with the outside air for too long after the outside air enters.

[0030] The present invention designs a closed raw material storage box. During discharge, when the discharge time is unknown, a circulation pipe is used to introduce outside air as the internal air pressure source for the box discharge. When the discharge is completed, the circulation pipe is closed, and the dry hot air supply mechanism, the heat pipe, and the air outlet pipe are opened. The efficient and short-time hot air flow supply method and the heating resistance heating method in the local range of the internal heating rod are used to efficiently and energy-savingly discharge the outside humid air remaining in the gap between the box and the raw materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0032] Figure 2 It is a schematic diagram of the explosion structure of the sealing cover and the box body of the present invention.

[0033] Figure 3 It is a schematic diagram of the cross-sectional structure of the box body of the present invention.

[0034] Figure 4 It is a schematic diagram of the box plane structure of the present invention.

[0035] In the figure: 1. Box body; 101. Raw material area; 102. Gas area; 2. Sealing cover; 3. Lower hopper; 4. Heating resistor; 5. Discharge pipe; 501. Discharge electric control valve; 6. Heat pipe; 7. Flow pipe; 8. Air outlet pipe; 9. Heating rod; 10. Distance sensor module; 11a. First electric control valve; 11b. Second electric control valve; 11c. Third electric control valve; 12. Humidity sensor module; 13. Dry hot air supply mechanism. DETAILED DESCRIPTION

[0036] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the accompanying drawings in the embodiments of the present invention.

[0037] Embodiment 1: The present invention designs a raw material drying and storage device for the production of pharmaceutical intermediates, which mainly includes the following contents:

[0038] Combination Figure 1 , Figure 2 , the lower hopper 3 is arranged at the bottom of the box body 1, and the lower hopper 3 is connected to the box body 1, the discharge pipe 5 is connected to the bottom of the lower hopper 3, and the discharge electric control valve 501 is arranged on one side of the discharge pipe 5. Raw materials are stored in the box body 1 to form a raw material area 101, and a gas area 102 is formed above the raw material area 101 in the box body 1. The sealing cover 2 is arranged at the top of the box body 1, and the distance sensor module 10 is fixedly arranged on the bottom side of the sealing cover 2. A plurality of heating rods 9 are fixedly arranged on the bottom side of the sealing cover 2. The lower side end of the heating rod 9 extends to the top area of ​​the lower hopper 3. A plurality of heating resistors 4 are arranged on the surface of the heating rod 9 at equal intervals from top to bottom. According to actual design needs, the resistance distribution of the heating resistors 4 can be designed. For example, the resistance values ​​of the plurality of heating resistors 4 on the heating rod 9 can be designed to be the same, or the resistance values ​​of the plurality of heating resistors 4 on the heating rod 9 can be designed to increase from top to bottom.

[0039] Combination Figure 3 , Figure 4, the heat pipe 6 is connected to one side of the box body 1 and communicated with the upper part of the gas area 102, the outlet pipe 8 is connected to the other side of the box body 1 and communicated with the upper part of the gas area 102, the horizontal positions of the heat pipe 6 and the outlet pipe 8 are higher than the highest position of the heating resistor 4 on the heating rod 9, the circulation pipe 7 is arranged on one side of the heat pipe 6, the output end of the dry hot gas supply mechanism 13 is communicated with one end of the heat pipe 6, a first electric control valve 11a is arranged on one side of the heat pipe 6, the first electric control valve 11a controls the on and off of the hot air flow in the heat pipe 6, the circulation pipe 7 is equipped with a second electric control valve 11b, and the outlet pipe 8 is equipped with a third electric control valve 11c. Based on the direction of the hot air flow injected from the heat pipe 6 to the box body 1: the position where the circulation pipe 7 is connected to the heat pipe 6 is located on the downstream side of the first electric control valve 11a, and a humidity sensor module 12 is installed on the inside of the box body 1. The humidity sensor module 12 is located in the gas area 102, and the humidity sensor module 12 is used to detect the humidity information of the gas area 102.

[0040] Embodiment 2: In the present invention, a method for using a raw material drying and storage device for producing pharmaceutical intermediates, the specific working principle is as follows:

[0041] First, open the sealing cover 2 and pour the pharmaceutical intermediate raw materials to be stored into the box body 1. A plurality of heating rods 9 are arranged inside the sealing cover 2. The heating rods 9 are energized and the sealing cover 2 is placed on the top of the box body 1. In this way, the heating rods 9 will extend into the interior of the box body 1 to heat and dry the pharmaceutical intermediate raw materials placed inside the box body 1.

[0042] Then, in the process of storing pharmaceutical intermediate raw materials, it is necessary to take out a part of the pharmaceutical intermediate raw materials from the box 1, open the discharge electric control valve 501 and the second electric control valve 11b, and the outside air flows into the box 1 from the circulation pipe 7, and the discharge pipe 5 discharges downward, and the pharmaceutical intermediate raw materials stored in the box 1 flows out from the discharge pipe 5. After the taking out is completed, the discharge electric control valve 501 and the second electric control valve 11b are closed, the dry hot air supply mechanism 13 is started, the first electric control valve 11a on the heat pipe 6 is opened, and the third electric control valve 11c on the outlet pipe 8 is opened. The dry hot air flow enters the interior of the box 1 from the heat pipe 6 to discharge the residual air in the gas area 102 of the box 1.

[0043] After a number of pharmaceutical intermediate raw materials are discharged from the discharge pipe 5, the distance sensor module 10 detects that the horizontal line of the pharmaceutical intermediate raw materials inside the box 1 has dropped, and controls the heating resistor 4 on the upper surface of the raw materials and within a certain depth range below it to work, so as to heat and dry the pharmaceutical intermediate raw materials on the upper surface and within a certain depth range below it, so as to prevent the pharmaceutical intermediate raw materials from being exposed to the outside air for too long and becoming damp and agglomerated.

[0044] The dry hot air flow enters the box 1 from the heat pipe 6, and the humidity sensor module 12 in the box 1 monitors the gas humidity parameter in the box 1 in real time. When the gas humidity parameter in the box 1 is lower than the minimum humidity reference value ψ preset by the system min When the time period below the reference value is greater than the reference time period t preset by the system, the dry hot air supply mechanism 13 stops, the first electrically controlled valve 11a of the heat pipe 6 is closed, and the third electrically controlled valve 11c of the air outlet pipe 8 is closed.

[0045] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A raw material drying and storage device for producing pharmaceutical intermediates, comprising a box (1) and a lower hopper (3), wherein the box (1) is connected to the lower hopper (3), a discharge pipe (5) is connected to the bottom of the lower hopper (3), a discharge electric control valve (501) is arranged at the position of the discharge pipe (5), raw materials are stored in the box (1) to form a raw material area (101), and a gas area (102) is formed on the upper side of the raw material area (101) in the inner cavity of the box (1), characterized in that: A sealing cover (2) is arranged on the top of the box body (1), a distance sensor module (10) is fixedly arranged on the bottom side of the sealing cover (2), a plurality of heating rods (9) are fixedly arranged on the bottom side of the sealing cover (2), and a plurality of heating resistors (4) are arranged on the surface of the heating rods (9) in order from top to bottom at equal intervals; One side of the upper part of the gas region (102) of the box (1) is connected to a heat pipe (6), the other side of the upper part of the gas region (102) of the box (1) is connected to an outlet pipe (8), the surface of the heat pipe (6) is connected to a flow pipe (7), a dry hot air supply mechanism (13) is arranged upstream of the heat pipe (6), the heat pipe (6) is arranged with a first electrically controlled valve (11a) for controlling the hot air flow, the flow pipe (7) is arranged with a second electrically controlled valve (11b), and the outlet pipe (8) is arranged with a third electrically controlled valve (11c); The inner wall of the box body (1) is provided with a humidity sensor module (12) located in the gas area (102).

2. The raw material drying and storage equipment for the production of pharmaceutical intermediates according to claim 1, characterized in that: The resistance values ​​of the multiple heating resistors (4) on the heating rod (9) are the same.

3. The raw material drying and storage equipment for the production of pharmaceutical intermediates according to claim 1, characterized in that: The resistance values ​​of the multiple heating resistors (4) on the heating rod (9) increase sequentially from top to bottom.

4. The raw material drying and storage equipment for the production of pharmaceutical intermediates according to claim 1, characterized in that: Taking the direction of hot air flow injected from the heat pipe (6) into the box (1) as a reference, the position where the flow pipe (7) is connected to the heat pipe (6) is located on the downstream side of the first electric control valve (11a).

5. The raw material drying and storage equipment for the production of pharmaceutical intermediates according to claim 1, characterized in that: The bottom of the box body (1) is connected to the top of the lower hopper (3), and the lower side end of the heating rod (9) extends to the top area of ​​the lower hopper (3).

6. The raw material drying and storage equipment for the production of pharmaceutical intermediates according to claim 1, characterized in that: Among the heating resistors (4) distributed on the heating rod (9), the horizontal position of the highest position heating resistor (4) is lower than the horizontal positions of the heat flux pipe (6) and the air outlet pipe (8).

7. A method for using a raw material drying and storage device for producing pharmaceutical intermediates, characterized in that: A raw material drying and storage device for producing pharmaceutical intermediates according to any one of claims 1 to 6, comprising the following steps: S1. Open the sealing cover (2), pour the pharmaceutical intermediate raw material to be stored into the box (1), and a plurality of heating rods (9) are provided inside the sealing cover (2). The heating rods (9) are energized to heat and dry the pharmaceutical intermediate raw material placed inside the box (1); S2. When a portion of the pharmaceutical intermediate raw material needs to be taken out from the box (1) during the process of storing the pharmaceutical intermediate raw material, the discharge electric control valve (501) and the second electric control valve (11b) are opened, and the outside air flows into the box (1) from the flow pipe (7), and the discharge pipe (5) discharges downward, and the pharmaceutical intermediate raw material stored in the box (1) flows out from the discharge pipe (5); S3. After the pharmaceutical intermediate raw material is taken out, the discharge electric control valve (501) and the second electric control valve (11b) are closed, the dry hot air supply mechanism (13) is started, the first electric control valve (11a) on the heat pipe (6) is opened, and the third electric control valve (11c) on the air outlet pipe (8) is opened, and the dry hot air flow enters the interior of the box (1) from the heat pipe (6) to discharge the residual air in the gas area (102) of the box (1); S4. Assume that the vertical distances between the plurality of heating resistors (4) of the heating rod (9) and the distance sensor module (10) are {L1, L2, L3, ..., L n }; When the distance sensing module (10) detects that the distance between the upper surface of the pharmaceutical intermediate material after the discharge operation is completed is Ls, it is determined that Ls is n }Relationship: Let Ls∈[L x-1 , L x ], then the control system drives L x-1 ~L x+m A heating resistor (4) within the range is used for heating; Among them, L x-1 ∈ {L1, L2, L3, ..., L n}, L x ∈ {L1, L2, L3, ..., L n}, L x+m ∈ {L1, L2, L3, ..., L n}; Among them, L x+m The m∝ distance sensing module (10) senses the distance Ls in real time; S5. The dry hot air flow enters the box (1) from the heat pipe (6). The humidity sensor module (12) in the box (1) monitors the gas humidity parameter in the box (1) in real time. When the gas humidity parameter in the box (1) is lower than the minimum humidity reference value ψ preset by the system min When the time period for which the temperature remains below the reference value is greater than a reference time period t preset by the system, the drying hot air supply mechanism (13) stops, the first electrically controlled valve (11a) of the heat pipe (6) is closed, and the third electrically controlled valve (11c) of the air outlet pipe (8) is closed.

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