Preparation and structure confirmation method and device of high-purity ganoderic acid

Abstract

The invention relates to the technical field of ganoderic acid, in particular to a preparation and structure confirmation method and device of high-purity ganoderic acid, and the technical scheme is that the device comprises a reaction kettle, a hopper, a radiator and a heater are respectively mounted in the reaction kettle, and a high-speed countercurrent chromatograph is mounted on the bottom end surface of the hopper through a discharge pipe; a crusher is mounted on the reaction kettle through a mounting frame, a screen is mounted in the crusher, a driving motor is mounted on the screen, and a crushing wheel is arranged on an output shaft of the driving motor; a mounting disc is mounted on the reaction kettle, a high-pressure pump and a carbon dioxide steel cylinder are respectively mounted on the mounting disc, and feeding pipes are respectively mounted on the top end surface of the reaction kettle in an embedded manner and are communicated with the reaction kettle. According to the method, the ganoderic acid quality problem during ganoderic acid detection is solved, the ganoderic acid can be optimally prepared, and the influence of internal temperature and pressure difference on the quality of the prepared ganoderic acid is avoided.

Description

Technical Field

[0001] The invention relates to the technical field of ganoderic acid, and in particular to a method and a device for preparing and confirming the structure of high-purity ganoderic acid. Background Art

[0002] Ganoderic acid is a secondary metabolite of Ganoderma lucidum, which has multiple pharmacological activities. Among them, Ganoderic acid T has been reported in the literature to have good anti-tumor effects in both in vitro cell experiments and in vivo mouse experiments. Pharmacological studies have shown that Ganoderic acid T can induce cancer cell apoptosis and inhibit cancer cell metastasis.

[0003] After extensive searching, the publication number is CN104725455B, which discloses a method for preparing ganoderic acid T. In the prior art, CN104725455B uses a high-speed countercurrent chromatograph to separate ganoderic acid T, and then uses a high-performance liquid chromatography to analyze and detect, collect, concentrate, and dry to separate and obtain ganoderic acid T. The method for preparing ganoderic acid T of the present invention is simple to operate, has little pollution, is low in cost, and has high yield and purity of ganoderic acid T.

[0004] However, when chromatographic analysis is directly used in the actual preparation of ganoderic acid, since the ganoderic material is not well processed and prepared, it is easy to cause more impurities in ganoderic acid, and the internal pressure and temperature cannot be adjusted during the preparation, which can easily affect the preparation and detection of ganoderic acid, so it still needs to be improved. Summary of the invention

[0005] The purpose of the present invention is to provide a method and device for preparing and confirming the structure of high-purity ganoderic acid, which can effectively solve the problems in the background technology.

[0006] To achieve the above object, the present invention provides the following technical solution: a device for preparing high-purity ganoderic acid, comprising a reaction kettle, wherein a hopper, a radiator and a heater are respectively installed in the reaction kettle;

[0007] A high-speed countercurrent chromatograph is installed on the bottom end surface of the hopper via a discharge pipe;

[0008] The reactor is provided with a pulverizer via a mounting frame, a screen is installed inside the reactor, a driving motor is installed on the screen, and a pulverizing wheel is provided on the output shaft of the driving motor;

[0009] The reactor is provided with a mounting plate, and a high-pressure pump and a carbon dioxide cylinder are respectively mounted on the mounting plate;

[0010] Preferably, a feed pipe is embedded and installed on the top surface of the reactor, and the feed pipe is connected to the reactor. A disperser is provided at one end of the feed pipe close to the inside of the reactor. The disperser is a conical structure with multiple guide grooves distributed on the surface for evenly dispersing the material added to the reactor.

[0011] When the above technical solution is adopted, the uniformity of material dispersion is improved: the disperser is a conical structure with guide grooves distributed on the surface, which can effectively disperse the material evenly in the reactor, so that the material can be more fully contacted during the reaction, thereby improving the reaction efficiency.

[0012] Preferably, a liquid outlet pipe is embedded and fixed on the bottom end surface of the high-speed countercurrent chromatograph, the liquid outlet pipe is connected to the high-speed countercurrent chromatograph, and a valve is installed on the liquid outlet pipe through a flange. A filter layer is provided inside the liquid outlet pipe and the discharge pipe, and the filter layer is a superimposed structure of multiple layers of filter screens with different pore sizes, which is used to further filter impurities in the separation liquid.

[0013] When the above technical solution is adopted, the liquid discharge can be flexibly controlled: the valve is installed through the flange, which is convenient for opening or closing the liquid discharge pipe at any time according to the needs, and the timing and flow rate of liquid discharge can be accurately controlled. The operation is convenient and the sealing is good. Efficient filtration of impurities: The filter layer with multiple layers of filter screens with different pore sizes can filter the separated liquid with multiple precisions and depths, effectively remove impurities of different particle sizes, and improve the purity of ganoderma lucidum acid.

[0014] Preferably, a discharging rack is embedded and fixed on the side end surface of the pulverizer, and the discharging rack is connected to the pulverizer.

[0015] When the above technical solution is adopted, the discharging rack can discharge the ganoderma lucidum materials processed in the crusher.

[0016] Preferably, an exhaust pipe is installed on the carbon dioxide cylinder, and the exhaust pipe is connected to the carbon dioxide cylinder, a valve is installed on the exhaust pipe through a flange, and a gas flow meter and a pressure stabilizing valve are also provided on the exhaust pipe. The gas flow meter is used to monitor the exhaust flow of carbon dioxide in real time, and the pressure stabilizing valve is used to stabilize the gas pressure in the exhaust pipe.

[0017] When the above technical solutions are adopted, the flow rate is precisely controlled: the gas flow meter monitors the carbon dioxide exhaust flow rate in real time, which is convenient for operators to adjust the flow rate according to the actual reaction requirements and ensure stable reaction conditions. Stable gas pressure: the pressure stabilizing valve can effectively maintain the gas pressure in the exhaust pipe, avoid the interference of pressure fluctuations on the reaction, and ensure the smooth progress of the reaction. Flexible control switch: the flange is installed with valves, which is easy to operate and has good sealing, making it easy to open or close the carbon dioxide supply in time.

[0018] Preferably, an extraction tube 1 and an extraction tube 2 are respectively installed on the high-pressure pump, and both the extraction tube 1 and the extraction tube 2 are connected to the high-pressure pump. Filter heads are provided at the ends of the extraction tube 1 and the extraction tube 2. The filter heads are made of porous ceramic material and are used to prevent impurities from entering the high-pressure pump.

[0019] When the above technical solution is adopted, impurity filtration protection: the porous ceramic filter head can effectively intercept impurities and prevent them from entering the high-pressure pump, thereby protecting the key components of the pump body, extending the service life and reducing the risk of equipment failure.

[0020] Preferably, a boost pipe and a carbon dioxide filling pipe are respectively embedded and fixed on the outer surface of the reactor, and the boost pipe and the carbon dioxide filling pipe are both connected to the reactor. The boost pipe and the carbon dioxide filling pipe are both provided with nozzles at one end close to the inside of the reactor, and the nozzles are rotary nozzles for evenly distributing the gas in the reactor.

[0021] When the above technical solution is adopted, the gas is evenly distributed: the rotary nozzle can evenly distribute the pressurized gas and carbon dioxide in the reactor in all directions and at multiple angles, ensuring a uniform reaction environment and improving reaction efficiency and product quality.

[0022] Preferably, a temperature sensor and a pressure sensor are installed in the reactor, and the temperature sensor and the pressure sensor are electrically connected to a controller installed outside the reactor, respectively, and the controller is also connected to the radiator, the heater and the high-pressure pump signal. The temperature sensor and the pressure sensor monitor the temperature and pressure in the reactor in real time. When the temperature or pressure exceeds the set range, the controller can automatically control the working state of the radiator, the heater or the high-pressure pump to maintain stable temperature and pressure conditions in the reactor, which is conducive to the smooth extraction process of ganoderma lucidum acid.

[0023] When the above technical solution is adopted, accurate real-time monitoring: temperature and pressure sensors grasp the temperature and pressure data in the reactor in real time, providing an accurate basis for the control of reaction conditions. Intelligent automatic control: the controller automatically controls the radiator, heater and high-pressure pump based on sensor feedback to ensure stable reaction conditions, ensure efficient and stable extraction of Ganoderma lucidum acid, and improve production efficiency and product quality.

[0024] Preferably, the high-speed countercurrent chromatograph is equipped with an online detection system, which includes a detector and a data processing module, and the detector is used to detect the purity, concentration and other parameters of the ganoderic acid separated from the high-speed countercurrent chromatograph in real time, and transmit the detection data to the data processing module for analysis and processing. When the detected parameters do not meet the preset standards, the operating parameters of the high-speed countercurrent chromatograph can be adjusted in time to ensure the high purity of the final product.

[0025] When the above technical solution is adopted, real-time monitoring: the online detection system can obtain the purity, concentration and other parameters of ganoderma lucidum in real time, so that the operator can grasp the separation situation in time. Precise control: the data processing module analyzes the data, and can adjust the chromatograph operating parameters in time when the parameters do not meet the preset standards to ensure the high purity of the product. Efficient production: avoid unqualified products caused by parameter deviation, reduce production losses, and improve production efficiency and quality stability.

[0026] A method for preparing and confirming high-purity ganoderic acid comprises the following steps:

[0027] S1. Raw material preparation and crushing: first, the ganoderma lucidum raw material is put into a crusher, a screen is installed in the crusher, and a driving motor on the screen drives a crushing wheel to rotate at high speed to crush the ganoderma lucidum raw material. The screen can ensure that the particle size of the crushed ganoderma lucidum raw material meets the requirements of subsequent reactions. The driving motor provides power, and the crushing wheel generates impact force and shear force through high-speed rotation to crush the ganoderma lucidum raw material into smaller particles, which is convenient for subsequent extraction in the reactor. The crushed raw material is discharged through a discharging rack connected to the crusher;

[0028] S2. Adding raw materials into the reaction vessel: The crushed Ganoderma lucidum raw materials are added into the reactor through a feed pipe. A conical disperser is arranged at one end of the feed pipe close to the inside of the reactor, and a plurality of guide grooves are distributed on the surface of the conical disperser. When the raw materials enter the reactor through the feed pipe, the disperser can evenly disperse the materials added into the reactor, so that the raw materials can fully contact with other substances in the reactor, thereby improving the reaction efficiency;

[0029] S3, adjusting the conditions in the reaction vessel: injecting pressurized gas and carbon dioxide gas into the reactor through the pressurizing pipe and the carbon dioxide filling pipe, and at the same time, using the temperature sensor and pressure sensor in the reactor to monitor the temperature and pressure in the reactor in real time;

[0030] S4. Carbon dioxide supply: Carbon dioxide gas in the carbon dioxide cylinder is extracted through the extraction pipe 1 on the high-pressure pump, and connected to the carbon dioxide filling pipe on the reactor through the extraction pipe 2, so as to supply carbon dioxide gas to the reactor, and the carbon dioxide gas is pressurized to a supercritical state by the high-pressure pump. The supercritical state is that the temperature and pressure are higher than the critical value, the density of carbon dioxide is close to that of liquid, and the viscosity and diffusion coefficient are close to those of gas;

[0031] S5. Preliminary separation of ganoderic acid: the mixed liquid after the reaction in the reactor enters the high-speed countercurrent chromatograph through the hopper and the discharge pipe. The high-speed countercurrent chromatograph is a chromatographic separation technology. It uses the special fluid dynamics phenomenon formed by the two-phase solvent system in the high-speed rotating spiral tube to make the sample be distributed between the two phases for many times, thereby realizing the separation of different components. In this process, ganoderic acid is preliminarily separated from other impurities, and the ganoderic acid can be analyzed and confirmed by the high-speed countercurrent chromatograph.

[0032] S6. Filtration and detection of separation liquid: The liquid separated from the high-speed countercurrent chromatograph is discharged through a liquid outlet pipe. A valve is installed on the liquid outlet pipe to control the discharge of the liquid. A filter layer with a superimposed structure of multiple layers of filter screens with different pore sizes is arranged inside the liquid outlet pipe to further filter out impurities in the separation liquid and improve the purity of Ganoderma lucidum acid. At the same time, the high-speed countercurrent chromatograph is equipped with an online detection system, including a detector and a data processing module. The detector is used to detect the purity, concentration and other parameters of Ganoderma lucidum acid separated from the high-speed countercurrent chromatograph in real time, and transmit the detection data to the data processing module for analysis and processing. When the detected parameters do not meet the preset standards, the operating parameters of the high-speed countercurrent chromatograph can be adjusted in time to ensure the high purity of the final product.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] Efficient material processing: the feed disperser disperses the material evenly and improves the reaction efficiency; the pulverizer discharge rack facilitates the discharge of processed materials.

[0035] Fine separation and filtration: The liquid outlet pipe and discharge pipe of the high-speed countercurrent chromatograph are equipped with multi-layer filter layers to effectively remove impurities; the valve controls the liquid outlet flexibly and accurately.

[0036] Stable gas supply: The exhaust pipe of the carbon dioxide cylinder is equipped with a flow meter, a pressure stabilizing valve and a valve to accurately control the flow, stabilize the pressure and enable flexible switching.

[0037] The equipment is well protected: the porous ceramic filter head at the end of the high-pressure pump extraction pipe intercepts impurities, protects the pump body and extends its service life.

[0038] Uniform reaction environment: The rotating nozzle of the reactor gas filling pipe makes the gas evenly distributed, improving the reaction efficiency and product quality.

[0039] Intelligent control of conditions: The temperature and pressure sensor works with the controller to monitor and automatically control the temperature and pressure of the reactor in real time to ensure stable extraction.

[0040] Real-time quality control: The high-speed countercurrent chromatograph online detection system monitors parameters in real time and makes timely adjustments if they do not meet the standards to ensure product purity and production efficiency, thereby confirming ganoderic acid. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 It is a side view structural schematic diagram of the present invention;

[0042] Figure 2 It is a schematic diagram of the main structure of the present invention;

[0043] Figure 3 It is a rear view structural schematic diagram of the present invention;

[0044] Figure 4It is a cross-sectional structural schematic diagram of the present invention;

[0045] Figure 5 It is a schematic diagram of the internal structure of the reactor of the present invention;

[0046] Figure 6 It is an enlarged structural schematic diagram of the pulverizer of the present invention;

[0047] Figure 7 It is a schematic diagram of the structure of the pulverizer of the present invention from a top view;

[0048] Figure 8 It is a schematic diagram of the process of the present invention.

[0049] In the figure: 1. Reactor; 101. Booster pipe; 102. Feed pipe; 103. Carbon dioxide filling pipe; 104. Discharge pipe; 105. High-speed countercurrent chromatograph; 106. Liquid outlet pipe; 107. Hopper; 108. Radiator; 109. Heater; 2. Crusher; 201. Mounting frame; 202. Discharge frame; 203. Crushing wheel; 204. Driving motor; 3. Mounting plate; 301. High-pressure pump; 302. Extraction pipe 1; 303. Extraction pipe 2; 304. Carbon dioxide cylinder. DETAILED DESCRIPTION

[0050] 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 described embodiments 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 creative work are within the scope of protection of the present invention.

[0051] Embodiment 1

[0052] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 and Figure 6As shown, an embodiment of the present invention is: a device for preparing high-purity ganoderic acid, comprising a reactor 1, wherein a hopper 107, a radiator 108 and a heater 109 are respectively installed in the reactor 1; a high-speed countercurrent chromatograph 105 is installed on the bottom end surface of the hopper 107 through a discharge pipe 104; a pulverizer 2 is installed on the reactor 1 through a mounting frame 201, a screen is installed inside, a driving motor 204 is installed on the screen, and a pulverizing wheel 203 is provided on the output shaft of the driving motor 204; a mounting plate 3 is installed on the reactor 1, and a high-pressure pump 301 and a carbon dioxide cylinder 304 are respectively installed on the mounting plate 3. The top surface of the reactor 1 is respectively embedded with a feed pipe 102, and the feed pipe 102 is connected to the reactor 1. A disperser is arranged at one end of the feed pipe 102 near the inside of the reactor 1. The disperser is a conical structure with a plurality of guide grooves distributed on the surface, which is used to evenly disperse the materials added to the reactor 1 and improve the uniformity of material dispersion: the disperser is a conical structure with guide grooves distributed on the surface, which can effectively evenly disperse the materials in the reactor 1, so that the materials can contact more fully during the reaction and improve the reaction efficiency. The side end surface of the pulverizer 2 is embedded with a discharging rack 202, and the discharging rack 202 is connected to the pulverizer 2. The discharging rack 202 can discharge the processed ganoderma lucidum materials in the pulverizer 2. The high-speed countercurrent chromatograph 105 is equipped with an online detection system, which includes a detector and a data processing module. The detector is used to detect the purity, concentration and other parameters of the ganoderma lucidum acid separated from the high-speed countercurrent chromatograph 105 in real time, and transmit the detection data to the data processing module for analysis and processing. When the detected parameters do not meet the preset standards, the operating parameters of the high-speed countercurrent chromatograph 105 can be adjusted in time to ensure the high purity of the final product. Real-time monitoring: The online detection system can obtain the purity, concentration and other parameters of ganoderma lucidum acid in real time, so that the operator can grasp the separation situation in time. Precise control: The data processing module analyzes the data and can adjust the chromatograph operating parameters in time when the parameters do not meet the preset standards to ensure the high purity of the product. Efficient production: Avoid unqualified products caused by parameter deviation, reduce production losses, and improve production efficiency and quality stability.

[0053] Embodiment 2

[0054] In order to facilitate the filtration of ganoderic acid, Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 and Figure 8As shown, an embodiment of the present invention is: a device for preparing high-purity ganoderic acid, comprising a reactor 1, wherein a hopper 107, a radiator 108 and a heater 109 are respectively installed in the reactor 1; a high-speed countercurrent chromatograph 105 is installed on the bottom end surface of the hopper 107 through a discharge pipe 104; a pulverizer 2 is installed on the reactor 1 through a mounting frame 201, a screen is installed inside, a driving motor 204 is installed on the screen, and a pulverizing wheel 203 is provided on the output shaft of the driving motor 204; a mounting plate 3 is installed on the reactor 1, and a high-pressure pump 301 and a carbon dioxide cylinder 304 are respectively installed on the mounting plate 3. The bottom end surface of the high-speed countercurrent chromatograph 105 is embedded with a liquid outlet pipe 106, which is connected to the high-speed countercurrent chromatograph 105, and a valve is installed on the liquid outlet pipe 106 through a flange. A filter layer is provided inside the liquid outlet pipe 106 and the discharge pipe 104. The filter layer is a multi-layer filter screen superposition structure with different apertures, which is used to further filter the impurities in the separated liquid and flexibly control the liquid discharge: the valve is installed through the flange, which is convenient to open or close the liquid outlet pipe 106 at any time as needed, accurately control the timing and flow rate of the liquid discharge, and is easy to operate and has good sealing. Efficiently filter impurities: The filter layer with multiple layers of filter screens with different apertures can filter the separated liquid with multiple precisions and depths, effectively remove impurities of different particle sizes, and improve the purity of ganoderma lucidum acid. A temperature sensor and a pressure sensor are installed in the reactor 1, and the temperature sensor and the pressure sensor are electrically connected to a controller installed outside the reactor 1, respectively, and the controller is also connected to the radiator 108, the heater 109 and the high-pressure pump 301 signal. The temperature sensor and pressure sensor monitor the temperature and pressure in the reactor 1 in real time. When the temperature or pressure exceeds the set range, the controller can automatically control the working state of the radiator 108, the heater 109 or the high-pressure pump 301 to maintain stable temperature and pressure conditions in the reactor 1, which is conducive to the smooth extraction of ganoderic acid. Accurate real-time monitoring: The temperature and pressure sensors grasp the temperature and pressure data in the reactor 1 in real time, providing an accurate basis for the regulation of reaction conditions. Intelligent automatic regulation: The controller automatically controls the radiator 108, the heater 109 and the high-pressure pump 301 based on the sensor feedback to ensure stable reaction conditions, ensure efficient and stable extraction of ganoderic acid, and improve production efficiency and product quality.

[0055] Embodiment 3

[0056] In order to further stabilize the internal pressure and temperature, avoid excessively high or low temperature and pressure, such as Figure 1 , Figure 5 , Figure 6 , Figure 7 and Figure 8As shown, an embodiment of the present invention is: a device for preparing high-purity ganoderic acid, comprising a reactor 1, wherein a hopper 107, a radiator 108 and a heater 109 are respectively installed in the reactor 1; a high-speed countercurrent chromatograph 105 is installed on the bottom end surface of the hopper 107 through a discharge pipe 104; a pulverizer 2 is installed on the reactor 1 through a mounting frame 201, a screen is installed inside, a driving motor 204 is installed on the screen, and a pulverizing wheel 203 is provided on the output shaft of the driving motor 204; a mounting plate 3 is installed on the reactor 1, and a high-pressure pump 301 and a carbon dioxide cylinder 304 are respectively installed on the mounting plate 3. An exhaust pipe is installed on the carbon dioxide cylinder 304, and the exhaust pipe is connected to the carbon dioxide cylinder 304. A valve is installed on the exhaust pipe through a flange. A gas flow meter and a pressure stabilizing valve are also provided on the exhaust pipe. The gas flow meter is used to monitor the discharge flow of carbon dioxide in real time, and the pressure stabilizing valve is used to stabilize the gas pressure in the exhaust pipe. The flow rate is precisely controlled: the gas flow meter monitors the discharge flow of carbon dioxide in real time, which is convenient for operators to adjust the flow rate according to actual reaction requirements and ensure stable reaction conditions. Stable gas pressure: The pressure stabilizing valve can effectively maintain the gas pressure in the exhaust pipe, avoid interference with the reaction caused by pressure fluctuations, and ensure the smooth progress of the reaction. Flexible control switch: The valve is installed on the flange, the switch operation is convenient, the sealing is good, and it is convenient to open or close the carbon dioxide supply in time. An extraction pipe 1 302 and an extraction pipe 2 303 are respectively installed on the high-pressure pump 301, and the extraction pipe 1 302 and the extraction pipe 2 303 are both connected to the high-pressure pump 301. Filter heads are provided at the ends of the extraction pipe 1 302 and the extraction pipe 2 303. The filter heads are made of porous ceramic material and are used to prevent impurities from entering the high-pressure pump 301. When the above technical solution is adopted, impurity filtering protection: the porous ceramic filter head can effectively intercept impurities and prevent them from entering the high-pressure pump 301, protect the key components of the pump body, extend the service life, and reduce the risk of equipment failure. A pressurizing pipe 101 and a carbon dioxide filling pipe 103 are respectively embedded and fixed on the outer surface of the reactor 1, and the pressurizing pipe 101 and the carbon dioxide filling pipe 103 are both connected to the reactor 1. The pressurizing pipe 101 and the carbon dioxide filling pipe 103 are both provided with nozzles at one end close to the inside of the reactor 1. The nozzles are rotary nozzles for evenly distributing the gas in the reactor 1. The gas is evenly distributed: the rotary nozzles can evenly distribute the pressurized gas and carbon dioxide in the reactor 1 in all directions and at multiple angles, ensuring a uniform reaction environment and improving reaction efficiency and product quality.

[0057] Embodiment 4

[0058] like Figure 1 and Figure 8 As shown, an embodiment of the present invention provides: a method for preparing and confirming high-purity ganoderic acid, comprising the following steps:

[0059] S1, raw material preparation and crushing: first, the ganoderma lucidum raw material is put into the crusher 2, and a screen is installed in the crusher 2. The driving motor 204 on the screen drives the crushing wheel 203 to rotate at high speed to crush the ganoderma lucidum raw material. The screen can ensure that the particle size of the crushed ganoderma lucidum raw material meets the requirements of the subsequent reaction. The driving motor 204 provides power, and the crushing wheel 203 generates impact force and shear force through high-speed rotation to crush the ganoderma lucidum raw material into smaller particles, which is convenient for subsequent extraction in the reactor 1. The crushed raw material is discharged through the discharging rack 202 connected to the crusher 2;

[0060] S2. Adding raw materials into the reaction vessel: The crushed Ganoderma lucidum raw materials are added into the reactor 1 through the feed pipe 102. A conical disperser is provided at one end of the feed pipe 102 close to the inside of the reactor 1. A plurality of guide grooves are distributed on the surface of the conical disperser. When the raw materials enter the reactor 1 through the feed pipe 102, the disperser can evenly disperse the materials added into the reactor 1, so that the raw materials can fully contact with other substances in the reactor 1, thereby improving the reaction efficiency.

[0061] S3, adjusting the conditions in the reaction vessel: injecting pressurized gas and carbon dioxide gas into the reactor 1 through the pressurizing pipe 101 and the carbon dioxide filling pipe 103, and at the same time, using the temperature sensor and pressure sensor in the reactor 1 to monitor the temperature and pressure in the reactor 1 in real time;

[0062] S4, carbon dioxide supply: the carbon dioxide gas in the carbon dioxide cylinder 304 is extracted through the extraction pipe 1 302 on the high-pressure pump 301, and connected to the carbon dioxide filling pipe 103 on the reactor 1 through the extraction pipe 2 303, so as to supply carbon dioxide gas to the reactor 1, and the carbon dioxide gas is pressurized to a supercritical state by the high-pressure pump 301. The supercritical state is when the temperature and pressure are higher than the critical value, the density of carbon dioxide is close to that of liquid, and the viscosity and diffusion coefficient are close to those of gas;

[0063] S5, preliminary separation of ganoderic acid: the mixed solution after the reaction in the reactor 1 enters the high-speed countercurrent chromatograph 105 through the hopper 107 and the discharge pipe 104. The high-speed countercurrent chromatograph 105 is a chromatographic separation technology, which utilizes the special fluid dynamics phenomenon formed by the two-phase solvent system in the high-speed rotating spiral tube to make the sample be distributed between the two phases for multiple times, thereby realizing the separation of different components. In this process, ganoderic acid is preliminarily separated from other impurities, and the ganoderic acid can be analyzed and confirmed by the high-speed countercurrent chromatograph 105;

[0064] S6. Filtration and detection of the separated liquid: the liquid separated from the high-speed countercurrent chromatograph 105 is discharged through the liquid outlet pipe 106. A valve is installed on the liquid outlet pipe 106 to control the discharge of the liquid. A filter layer with a superimposed structure of multiple layers of filter screens with different pore sizes is arranged inside the liquid outlet pipe 106 to further filter out impurities in the separated liquid and improve the purity of ganoderma acid. At the same time, the high-speed countercurrent chromatograph 105 is equipped with an online detection system, including a detector and a data processing module. The detector is used to detect the purity, concentration and other parameters of the ganoderma acid separated from the high-speed countercurrent chromatograph 105 in real time, and transmit the detection data to the data processing module for analysis and processing. When the detected parameters do not meet the preset standards, the operating parameters of the high-speed countercurrent chromatograph 105 can be adjusted in time to ensure the high purity of the final product.

Claims

1. A device for preparing high-purity ganoderic acid, comprising a reaction kettle (1), wherein a hopper (107), a radiator (108) and a heater (109) are respectively installed in the reaction kettle (1), characterized in that: A high-speed countercurrent chromatograph (105) is installed on the bottom end surface of the hopper (107) through a discharge pipe (104); The reaction kettle (1) is provided with a pulverizer (2) via a mounting frame (201), a screen is installed inside the reaction kettle, a driving motor (204) is installed on the screen, and a pulverizing wheel (203) is provided on the output shaft of the driving motor (204); The reaction kettle (1) is provided with a mounting plate (3), and a high-pressure pump (301) and a carbon dioxide cylinder (304) are respectively mounted on the mounting plate (3).

2. The device for preparing high-purity ganoderic acid according to claim 1, characterized in that: A feed pipe (102) is embedded and installed on the top surface of the reactor (1), and the feed pipe (102) is connected to the reactor (1). A disperser is arranged at one end of the feed pipe (102) close to the inside of the reactor (1). The disperser is a conical structure with a plurality of guide grooves distributed on the surface, which is used to evenly disperse the material added to the reactor (1).

3. The device for preparing high-purity ganoderic acid according to claim 1, characterized in that: A liquid outlet pipe (106) is embedded and fixed in the bottom end surface of the high-speed countercurrent chromatograph (105), the liquid outlet pipe (106) is connected to the high-speed countercurrent chromatograph (105), and a valve is installed on the liquid outlet pipe (106) through a flange. A filter layer is arranged inside the liquid outlet pipe 106 and the discharge pipe 104, and the filter layer is a superimposed structure of multiple layers of filter screens with different pore sizes, which is used to further filter impurities in the separation liquid.

4. The device for preparing high-purity ganoderic acid according to claim 1, characterized in that: A discharging frame (202) is embedded and fixed on the side end surface of the pulverizer (2), and the discharging frame (202) is in communication with the pulverizer (2).

5. The device for preparing high-purity ganoderic acid according to claim 1, characterized in that: An exhaust pipe is installed on the carbon dioxide cylinder (304), and the exhaust pipe is connected to the carbon dioxide cylinder (304). A valve is installed on the exhaust pipe via a flange. A gas flow meter and a pressure stabilizing valve are also provided on the exhaust pipe. The gas flow meter is used to monitor the exhaust flow of carbon dioxide in real time, and the pressure stabilizing valve is used to stabilize the gas pressure in the exhaust pipe.

6. The device for preparing high-purity ganoderic acid according to claim 1, characterized in that: The high-pressure pump (301) is respectively provided with an extraction pipe 1 (302) and an extraction pipe 2 (303), and both the extraction pipe 1 (302) and the extraction pipe 2 (303) are connected to the high-pressure pump (301), and the ends of the extraction pipe 1 (302) and the extraction pipe 2 (303) are provided with filter heads, and the filter heads are made of porous ceramic material and are used to prevent impurities from entering the high-pressure pump (301).

7. The device for preparing high-purity ganoderic acid according to claim 1, characterized in that: A pressurizing pipe (101) and a carbon dioxide filling pipe (103) are respectively embedded and fixed on the outer surface of the reactor (1), and the pressurizing pipe (101) and the carbon dioxide filling pipe (103) are both connected to the reactor (1). A nozzle is provided at one end of the pressurizing pipe (101) and the carbon dioxide filling pipe (103) close to the inside of the reactor (1), and the nozzle is a rotary nozzle for evenly distributing the gas in the reactor (1).

8. The device for preparing high-purity ganoderic acid according to claim 1, characterized in that: The reactor (1) is equipped with a temperature sensor and a pressure sensor, and the temperature sensor and the pressure sensor are respectively electrically connected to a controller installed outside the reactor (1), and the controller is also connected to the radiator (108), the heater (109) and the high-pressure pump (301) by signal. The temperature sensor and the pressure sensor monitor the temperature and pressure in the reactor (1) in real time. When the temperature or pressure exceeds the set range, the controller can automatically control the working state of the radiator (108), the heater (109) or the high-pressure pump (301), so that the temperature and pressure conditions in the reactor (1) are kept stable, which is conducive to the smooth extraction process of ganoderma lucidum acid.

9. The device for preparing high-purity ganoderic acid according to claim 1, characterized in that: The high-speed countercurrent chromatograph (105) is equipped with an online detection system, which includes a detector and a data processing module. The detector is used to detect the purity, concentration and other parameters of the ganoderic acid separated from the high-speed countercurrent chromatograph (105) in real time, and transmit the detection data to the data processing module for analysis and processing. When the detected parameters do not meet the preset standards, the operating parameters of the high-speed countercurrent chromatograph (105) can be adjusted in time to ensure the high purity of the final product.

10. A method for preparing and confirming high-purity ganoderic acid, characterized in that: The following steps are involved: S1. Raw material preparation and crushing: first, the ganoderma lucidum raw material is put into a crusher (2). A screen is installed in the crusher (2). The driving motor (204) on the screen drives the crushing wheel (203) to rotate at high speed to crush the ganoderma lucidum raw material. The screen can ensure that the particle size of the crushed ganoderma lucidum raw material meets the requirements of subsequent reactions. The driving motor (204) provides power. The crushing wheel (203) generates impact force and shear force through high-speed rotation to crush the ganoderma lucidum raw material into smaller particles, which is convenient for subsequent extraction in the reactor (1). The crushed raw material is discharged through a discharging rack (202) connected to the crusher (2); S2. Adding raw materials into the reaction vessel: The crushed ganoderma lucidum raw materials are added into the reaction kettle (1) through the feeding pipe (102). A conical disperser is arranged at one end of the feeding pipe (102) close to the inside of the reaction kettle (1). A plurality of guide grooves are distributed on the surface of the conical disperser. When the raw materials enter the reaction kettle (1) through the feeding pipe (102), the disperser can evenly disperse the materials added into the reaction kettle (1), so that the raw materials can fully contact with other substances in the reaction kettle (1), thereby improving the reaction efficiency. S3, adjusting the conditions in the reaction vessel: injecting pressurized gas and carbon dioxide gas into the reactor (1) through the pressurizing pipe (101) and the carbon dioxide filling pipe (103), and at the same time, using the temperature sensor and pressure sensor in the reactor (1) to monitor the temperature and pressure in the reactor (1) in real time; S4. Carbon dioxide supply: The carbon dioxide gas in the carbon dioxide cylinder (304) is extracted through the extraction pipe 1 (302) on the high-pressure pump (301), and connected to the carbon dioxide filling pipe (103) on the reactor (1) through the extraction pipe 2 (303), so as to supply carbon dioxide gas to the reactor (1), and the carbon dioxide gas is pressurized to a supercritical state by the high-pressure pump (301). The supercritical state is when the temperature and pressure are higher than the critical value, the density of carbon dioxide is close to that of liquid, and the viscosity and diffusion coefficient are close to those of gas; S5. Preliminary separation of ganoderic acid: the mixed solution after the reaction in the reactor (1) enters the high-speed countercurrent chromatograph (105) through the hopper (107) and the discharge pipe (104). The high-speed countercurrent chromatograph (105) is a chromatographic separation technology. It uses the special fluid dynamics phenomenon formed by the two-phase solvent system in the high-speed rotating spiral tube to make the sample be distributed between the two phases for multiple times, thereby achieving the separation of different components. In this process, ganoderic acid is preliminarily separated from other impurities, and the ganoderic acid can be analyzed and confirmed by the high-speed countercurrent chromatograph (105); S6. Filtration and detection of the separated liquid: The liquid separated from the high-speed countercurrent chromatograph (105) is discharged through the liquid outlet pipe (106). A valve is installed on the liquid outlet pipe (106) to control the discharge of the liquid. A filter layer with a superimposed structure of multiple layers of filter screens with different pore sizes is arranged inside the liquid outlet pipe (106) to further filter out impurities in the separated liquid and improve the purity of ganoderma lucidic acid. At the same time, the high-speed countercurrent chromatograph (105) is equipped with an online detection system, including a detector and a data processing module. The detector is used to detect the purity, concentration and other parameters of the ganoderma lucidic acid separated from the high-speed countercurrent chromatograph (105) in real time, and transmit the detection data to the data processing module for analysis and processing. When the detected parameters do not meet the preset standards, the operating parameters of the high-speed countercurrent chromatograph (105) can be adjusted in time to ensure the high purity of the final product.

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