Silybin separation and purification device with spray drying mechanism

By introducing a spray drying mechanism into the silybin separation and purification device, combined with a heat recovery and material preheating system, the problem of high energy consumption was solved, and an efficient and low-cost silybin purification process was achieved.

CN223392899UActive Publication Date: 2025-09-30JIANGSU JIANJIA PHARM IND CORP LTD
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Patent Information

Application Number
CN202422762280.1
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-11-13
Publication Date
2025-09-30
Estimated Expiration
2034-11-13

AI Technical Summary

Technical Problem

The existing silybin separation and purification equipment has high energy consumption and serious heat energy waste in the spray drying process, and lacks a preheating system for the material temperature, resulting in high operating costs.

Method used

A silybin separation and purification device with a spray drying mechanism was designed. The device used a macroporous resin chromatography column, an evaporation crystallization kettle, and a spray drying mechanism. A high-pressure atomizing rotary nozzle and an insulation tank were combined to achieve heat recovery and material preheating. A heater and a fan system provided a clean hot air flow, and a filter air inlet and filter plates were provided to remove impurities.

Benefits of technology

It achieves efficient heat recovery, improves drying efficiency, ensures material purity, reduces energy consumption and improves the purity of silybin.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to the field of silibinin production, and discloses a silibinin separation and purification device with a spray drying mechanism, which comprises a macroporous resin chromatographic column and an evaporative crystallization kettle, the evaporative crystallization kettle is arranged on the right side of the macroporous resin chromatographic column, and the spray drying mechanism is arranged between the macroporous resin chromatographic column and the evaporative crystallization kettle. According to the silibinin separation and purification device with the spray drying mechanism, the spray drying mechanism is arranged, high-temperature waste gas upwards passes through a drainage pipe from a waste gas opening and is circularly introduced into the heat preservation tank, crystals with dropping liquid in the material box are preheated, and therefore heat energy is recycled, the heat preservation tank is made of an aluminum-plastic film plate material, and the outer portion of the heat preservation tank is coated with heat preservation cotton; according to the spray drying device, crystals entering the spray drying mechanism can be continuously preheated, the problem of heat energy waste is solved, the drying efficiency is greatly improved through efficient heat energy recovery, and the problems that in the spray drying process, energy consumption is high, and the drying efficiency is affected are solved.
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Description

Technical Field

[0001] The utility model relates to the technical field of silibinin, in particular to a silibinin separation and purification device with a spray drying mechanism. Background Art

[0002] Silybin is a key ingredient extracted from milk thistle, exhibiting promising pharmacological effects such as liver protection and antioxidant properties. Separation and purification are key steps in the preparation of silybin, which primarily involves chromatographic separation, evaporative crystallization, and spray drying. In the initial treatment, the silybin solution undergoes initial purification through adsorption and elution on a chromatography column, removing non-target components such as pigments and impurities. Next, in an evaporative crystallization reactor, temperature and pressure are controlled to gradually precipitate silybin from the solution into crystals. To facilitate storage and further application of silybin, the crystallized solution is spray-dried to convert the crystals into a fine powder.

[0003] Existing silybin separation and purification systems on the market suffer from high energy consumption during the spray drying process, particularly due to the use of high-temperature airflow. This wastes a significant amount of heat energy during the drying process and fails to fully recycle it. High-temperature exhaust gases generated during the drying process are often directly discharged without recycling, yet they still contain a significant amount of heat. Furthermore, the material lacks a preheating system before entering the spray drying stage, requiring it to be heated directly to a high temperature to meet drying requirements. This further increases overall energy consumption and leads to high operating costs.

[0004] Therefore, there is an urgent need for a silybin separation and purification device with a spray drying mechanism to solve the above problems. Utility Model Content

[0005] The purpose of the utility model is to provide a silybin separation and purification device with a spray drying mechanism to solve the problem of high energy consumption and affected drying efficiency proposed in the above background technology.

[0006] To achieve the above-mentioned object, the utility model provides the following technical solution: a silybin separation and purification device with a spray drying mechanism, comprising a macroporous resin chromatography column and an evaporation crystallization kettle, an evaporation crystallization kettle being provided on the right side of the macroporous resin chromatography column, and a spray drying mechanism being provided between the macroporous resin chromatography column and the evaporation crystallization kettle; a fixed seat is surrounded on the top of the spray drying mechanism, a high-pressure atomizing rotary nozzle is installed at the middle position of the top of the spray drying mechanism, an insulation tank is fixedly connected to the right side of the fixed seat, a material box is placed in the insulation tank, a material pump is installed between the insulation tank and the high-pressure atomizing rotary nozzle, a powder discharge pump is installed at the discharge port at the bottom end of the spray drying mechanism, a discharge barrel is fixed on the right side of the spray drying mechanism, a container is provided below the discharge barrel, the powder discharge pump is upwardly connected to the discharge barrel, an exhaust port is provided on the top of the discharge barrel, a drainage pipe is connected between the exhaust port and the insulation tank, an exhaust hole is opened on the top of the insulation tank, and a bushing is provided on the outside of the spray drying mechanism.

[0007] As a further technical solution of the present invention, the heat preservation tank is made of aluminum-plastic film material and is coated with heat preservation cotton on the outside.

[0008] As a further technical solution of the present invention, the material pump and the material box are connected by a pipeline, and the outside of the pipeline is coated with thermal insulation cotton.

[0009] As a further technical solution of the present invention, a heater is fixedly connected to the left side wall of the fixing seat, a fan is installed on the top of the heater, and the fan outlet pipe passes through the fixing seat and is connected to the inside of the spray drying mechanism.

[0010] As a further technical solution of the present invention, a temperature control system is installed at the heater, and the temperature control system is a disc-shaped component with an open bottom.

[0011] As a further technical solution of the present invention, a mounting port is provided at the bottom end of the heater, and a filter air inlet cylinder is connected to the mounting port through a threaded connection. A filter plate is installed in the filter air inlet cylinder, and an air inlet groove matching the size of the filter plate is opened at the bottom end of the filter air inlet cylinder.

[0012] As a further technical solution of the present invention, buckles are fixed on both sides of the filter plate, and two groups of clamping seats are fixedly connected to the inner wall of the filter air inlet cylinder, and the buckles are embedded in the clamping seats.

[0013] As a further technical solution of the present invention, a preceding feed port is installed at the macroporous resin chromatography column, the macroporous resin chromatography column and the evaporation crystallization kettle are connected by a pipeline, the evaporation crystallization kettle and the material box are connected by a pipeline, each pipeline in the device is installed with a check valve, and the steam inlet of the evaporation crystallization kettle is connected to the preceding steam generator.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows: the silybin separation and purification device with a spray drying mechanism not only realizes efficient heat energy recovery, improves drying efficiency, and avoids the decrease in material purity caused by air impurities during the drying process, but also realizes a more efficient process from extraction to fine purification, resulting in higher purity;

[0015] By providing a spray drying mechanism and adding a drainage pipe to the spray drying mechanism, the high-temperature exhaust gas generated is circulated upward through the drainage pipe from the exhaust port and introduced into the insulation tank, preheating the crystals with dripping liquid in the material box, thereby realizing heat energy recovery. The insulation tank is made of aluminum-plastic film material and is coated with insulation cotton on the outside, which can ensure that the crystals entering the spray drying mechanism are continuously preheated, solve the problem of heat energy waste, and greatly improve the drying efficiency through efficient heat energy recovery;

[0016] The heater, fan, filter air inlet, filter plate, holder, and buckle are provided. The heater sends a clean, high-temperature hot air flow into the spray drying mechanism through the fan. At the bottom end of the heater, the filter air inlet is threadedly connected to the installation port. The filter air inlet is installed with a group of detachable and cleanable filter plates through the holder and the buckle. The air flow entering the fan is removed by the filter plates, thereby avoiding the decrease in material purity due to air impurities during the drying process and ensuring the final purity of the silybin material.

[0017] The invention is provided with a macroporous resin chromatography column, an evaporation crystallization kettle, a spray drying mechanism, and a container. The macroporous resin chromatography column separates silibinin from other impurities by regulating the flow rate and polarity of different solvents, thereby obtaining a silibinin solution with higher purity and removing impurities such as pigments and fats. The purified solution enters the evaporation crystallization kettle, where silibinin crystals are precipitated by evaporation and concentration. Crystal droplets are pumped into a material box and fed into a high-pressure atomizing rotary nozzle by a material pump. A heater guides the heated air flow into the spray drying mechanism. The high-pressure atomizing rotary nozzle rotates at a high speed, and the silibinin is converted into a fine powder through spray drying. The process from extraction to fine purification is more efficient and the purity is higher. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is a schematic diagram of the front cross-sectional structure of the present utility model;

[0019] Figure 2 This is a schematic diagram of the front cross-sectional structure of the spray drying mechanism of the present invention;

[0020] Figure 3 This is a schematic diagram of the front view structure of the filter plate of the present invention;

[0021] Figure 4 This is a front view structural diagram of the evaporation crystallization kettle of the present utility model.

[0022] In the figure: 1. Pre-sequence feed port; 2. Macroporous resin chromatography column; 3. Spray drying mechanism; 4. High-pressure atomizing rotary nozzle; 5. Feed pump; 6. Feed box; 7. Insulation tank; 8. Evaporation crystallization kettle; 9. Drainage pipe; 10. Exhaust port; 11. Discharge barrel; 12. Container; 13. Heater; 14. Fixing seat; 15. Bushing; 16. Filter air inlet; 17. Fan; 18. Powder discharge pump; 19. Exhaust hole; 20. Holder; 21. Buckle; 22. Filter plate; 23. Air inlet slot; 24. Installation port; 25. Temperature control system. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0024] See also Figure 1-4 The utility model provides an embodiment: a silybin separation and purification device with a spray drying mechanism, comprising a macroporous resin chromatography column 2 and an evaporation crystallization kettle 8, the evaporation crystallization kettle 8 is arranged on the right side of the macroporous resin chromatography column 2, and a spray drying mechanism is arranged between the macroporous resin chromatography column 2 and the evaporation crystallization kettle 8; the top of the spray drying mechanism is surrounded by a fixed seat 14, a high-pressure atomizing rotary nozzle 4 is installed at the middle position of the top of the spray drying mechanism 3, a heat preservation tank 7 is fixedly connected to the right side of the fixed seat 14, a material box 6 is placed in the heat preservation tank 7, and a material box 6 is placed between the heat preservation tank 7 and the high-pressure atomizing rotary nozzle 4. A material pump 5 is installed, a powder discharge pump 18 is installed at the bottom discharge port of the spray drying mechanism 3, a discharge cylinder 11 is fixed to the right side of the spray drying mechanism 3, a container 12 is provided below the discharge cylinder 11, the powder discharge pump 18 is upwardly connected to the discharge cylinder 11, an exhaust port 10 is provided at the top of the discharge cylinder 11, a drainage pipe 9 is connected between the exhaust port 10 and the insulation tank 7, an exhaust hole 19 is provided at the top of the insulation tank 7, a sleeve 15 is provided on the outside of the spray drying mechanism 3, the insulation tank 7 is made of aluminum-plastic film material, and the outside is covered with insulation cotton, the material pump 5 and the material box 6 are connected by a pipeline, and the outside of the pipeline is covered with insulation cotton;

[0025] Specifically, if Figure 1 、 Figure 2 、 Figure 3 and Figure 4As shown, the purified solution is concentrated by evaporation to precipitate silybin crystals, and the crystal droplets are pumped into the material box 6 and sent to the high-pressure atomizing rotary nozzle 4 by the material pump 5. The heater 13 introduces the heated airflow into the spray drying mechanism 3. The high-pressure atomizing rotary nozzle 4 rotates at a high speed and is converted into a fine powder by spray drying. After the powder is discharged, it enters the discharge barrel 11. The high-temperature powder falls into the container 12 from the bottom of the discharge barrel 11, and the high-temperature exhaust gas is circulated upward from the exhaust port 10 through the drainage pipe 9 and introduced into the insulation tank 7 to preheat the crystals with droplets in the material box 6, thereby realizing heat energy recovery. The insulation tank 7 is made of aluminum-plastic film material and is coated with insulation cotton on the outside, which can ensure that the crystals entering the spray drying mechanism 3 are continuously preheated, solve the problem of heat energy waste, and greatly improve the drying efficiency through efficient heat energy recovery.

[0026] The left side wall of the fixed seat 14 is fixedly connected to the heater 13, and a fan 17 is installed on the top of the heater 13. The air outlet pipe of the fan 17 passes through the fixed seat 14 and is connected to the inside of the spray drying mechanism 3. A temperature control system 25 is installed at the heater 13. The temperature control system 25 is a disc-shaped component with an open bottom. A mounting port 24 is provided at the bottom end of the heater 13. The mounting port 24 is connected to the filter air inlet cylinder 16 through a thread. A filter plate 22 is assembled in the filter air inlet cylinder 16. An air inlet slot 23 matching the size of the filter plate 22 is provided at the bottom end of the filter air inlet cylinder 16. Buckles 21 are respectively fixed on both sides of the filter plate 22. Two sets of clamps 20 are fixedly connected to the inner wall of the filter air inlet cylinder 16, and the clamps 21 are embedded in the clamps 20.

[0027] Specifically, if Figure 1 、 Figure 2 and Figure 3 As shown, the heater 13 delivers a clean, high-temperature hot air flow into the spray drying mechanism 3 through the fan 17. At the bottom end of the heater 13, the filter air inlet cylinder 16 is threadedly connected through the mounting port 24. The filter air inlet cylinder 16 is mounted with a set of detachable and cleanable filter plates 22 through the fastening connection of the clamping seat 20 and the buckle 21. The air flow entering the fan 17 is removed by the filter plates 22 to avoid the decrease in material purity due to air impurities during the drying process, thereby ensuring the final purity of the silybin material.

[0028] A pre-process feed port 1 is installed at the macroporous resin chromatography column 2, the macroporous resin chromatography column 2 and the evaporation crystallization kettle 8 are connected by a pipeline, the evaporation crystallization kettle 8 and the material box 6 are connected by a pipeline, each pipeline in the device is equipped with a check valve, and the steam inlet of the evaporation crystallization kettle 8 is connected to the pre-process steam generator;

[0029] Specifically, if Figure 1 、 Figure 2 and Figure 4As shown, the macroporous resin chromatography column 2 separates silibinin from other impurities by regulating the flow rate and polarity of different solvents to obtain a silibinin solution with higher purity, removing impurities such as pigments and fats. The purified solution enters the evaporation crystallization kettle 8, where silibinin crystals are precipitated by evaporation and concentration. The crystal droplets are pumped into the material box 6 and fed into the high-pressure atomizing rotary nozzle 4 by the material pump 5. The heater 13 guides the heated air flow into the spray drying mechanism 3, and the dried silibinin fine powder enters the container 12. The process from extraction to fine purification is more efficient and the purity is higher.

[0030] Working principle: The device is divided into three processes: fine separation, evaporation crystallization and spray drying. The macroporous resin chromatography column 2 separates silybin from other impurities by regulating the flow rate and polarity of different solvents to obtain a higher purity silybin solution, removing impurities such as pigments and fats. The purified solution enters the evaporation crystallization kettle 8, and silybin crystals are precipitated by evaporation and concentration. They are sent to the material box 6 and then sent to the high-pressure atomizing rotary nozzle 4 by the material pump 5. The heater 13 introduces the heated air flow into the spray drying mechanism 3. The high-pressure atomizing rotary nozzle 4 rotates at a high speed and is converted into a fine powder through spray drying. After the powder is discharged, it enters the discharge barrel 11. The high-temperature powder falls from the bottom of the discharge barrel 11 into the container 12, and the high-temperature exhaust gas is circulated upward from the exhaust port 10 through the drainage pipe 9 and introduced into the insulation tank 7 to preheat the crystals with dripping liquid in the material box 6. The dried silybin fine powder enters the container 12.

Claims

1. A silybin separation and purification device with a spray drying mechanism, comprising a macroporous resin chromatography column (2) and an evaporation crystallization kettle (8), characterized in that: An evaporation crystallization kettle (8) is provided on the right side of the macroporous resin chromatography column (2), and a spray drying mechanism is provided between the macroporous resin chromatography column (2) and the evaporation crystallization kettle (8); The top of the spray drying mechanism is surrounded by a fixed seat (14), a high-pressure atomizing rotary nozzle (4) is installed at the middle position of the top of the spray drying mechanism (3), a heat preservation tank (7) is fixedly connected to the right side of the fixed seat (14), a material box (6) is placed in the heat preservation tank (7), a material pump (5) is installed between the heat preservation tank (7) and the high-pressure atomizing rotary nozzle (4), a powder discharge pump (18) is installed at the discharge port at the bottom end of the spray drying mechanism (3), a discharge barrel (11) is fixed on the right side of the spray drying mechanism (3), a container (12) is provided below the discharge barrel (11), the powder discharge pump (18) is connected upward to the discharge barrel (11), an exhaust port (10) is provided at the top of the discharge barrel (11), a drainage pipe (9) is connected between the exhaust port (10) and the heat preservation tank (7), an exhaust hole (19) is opened at the top of the heat preservation tank (7), and a bushing (15) is provided on the outside of the spray drying mechanism (3).

2. The silybin separation and purification device with a spray drying mechanism according to claim 1, characterized in that: The heat-insulating tank (7) is made of aluminum-plastic film material and is coated with heat-insulating cotton on the outside.

3. The silybin separation and purification device with a spray drying mechanism according to claim 1, characterized in that: The material pump (5) and the material box (6) are connected via a pipeline, and the outside of the pipeline is coated with thermal insulation cotton.

4. The silybin separation and purification device with a spray drying mechanism according to claim 1, characterized in that: A heater (13) is fixedly connected to the left side wall of the fixing seat (14), a fan (17) is installed on the top of the heater (13), and an air outlet pipe of the fan (17) passes through the fixing seat (14) and is connected to the interior of the spray drying mechanism (3).

5. The silybin separation and purification device with a spray drying mechanism according to claim 4, characterized in that: A temperature control system (25) is installed at the heater (13), and the temperature control system (25) is a disc-shaped component with an open bottom.

6. The silybin separation and purification device with a spray drying mechanism according to claim 4, characterized in that: The bottom end of the heater (13) is provided with a mounting opening (24), and the mounting opening (24) is connected to a filter air inlet cylinder (16) via a threaded connection. A filter plate (22) is installed in the filter air inlet cylinder (16), and an air inlet slot (23) matching the size of the filter plate (22) is provided at the bottom end of the filter air inlet cylinder (16).

7. The silybin separation and purification device with a spray drying mechanism according to claim 6, characterized in that: Buckles (21) are fixed on both sides of the filter plate (22), and two groups of clamping seats (20) are fixedly connected to the inner wall of the filter air inlet cylinder (16), and the buckles (21) are embedded in the clamping seats (20).

8. The silybin separation and purification device with a spray drying mechanism according to claim 1, characterized in that: The macroporous resin chromatography column (2) is provided with a pre-sequence feed port (1), the macroporous resin chromatography column (2) and the evaporation crystallization kettle (8) are connected via a pipeline, the evaporation crystallization kettle (8) and the material box (6) are connected via a pipeline, each pipeline in the device is provided with a check valve, and the steam inlet of the evaporation crystallization kettle (8) is connected to the pre-sequence steam generator.