A multi-stage cryogenic condensation high vacuum solvent capture system

Abstract

The utility model relates to a kind of multistage low-temperature condensation high-vacuum solvent trapping systems, including high-vacuum cavity, multistage gradient cold trap system, high-vacuum unit and intelligent control system, high-vacuum cavity is equipped with sample container multilayer support, multiple rotary trays are equipped on sample container multilayer support, material container is equipped on rotary tray, the below of rotary tray is equipped with multiple heaters of asymmetric distribution, heater is connected with intelligent control system respectively;Multistage gradient cold trap system includes at least two levels of series connection setting cold trap assembly, the working temperature of each level cold trap is gradually reduced from the cold trap assembly of the side close to high-vacuum cavity to the cold trap assembly of the side close to high-vacuum unit;Each level cold trap is connected with matched refrigerator unit, and the bottom of each level cold trap is connected with matched solvent tank.The utility model realizes efficient solvent trapping and recovery, significantly improves trapping efficiency, protects sample activity, and improves automation degree.

Description

Technical Field

[0001] This utility model relates to the field of biomedical experimental equipment technology, and in particular to a multi-stage low-temperature condensation high-vacuum solvent collection system. Background Technology

[0002] In the research and development and production of biopharmaceutical products, such as proteins, peptides, vaccines, and nucleic acid drugs, large amounts of volatile organic solvents, such as methanol, ethanol, ethylene glycol, acetone, and dichloromethane, are frequently used in processes such as solvent replacement, concentration, and post-processing of chemical polymerization reactions. These processes must be carried out in low-temperature, vacuum environments to lower the boiling points of the materials and prevent the deactivation and contamination of heat-sensitive substances.

[0003] Currently, the solvent capture method used in existing technologies is the single-stage cryogenic cold trap vacuum capture method. Its basic principle is to reduce the boiling point of the solvent by reducing the system pressure, thereby achieving rapid evaporation of the solvent at a lower temperature, and then capturing the evaporated solvent through a condenser to achieve the purpose of solvent recovery.

[0004] Existing cold trap condensation collection devices typically consist of a vacuum chamber, a heater, a vacuum pump, and a single-stage cold trap. However, these devices have the following drawbacks: (1) Limited capture efficiency: When a large amount of various organic solvents (such as acetonitrile and methanol) are concentrated, the defects such as the single-stage cold trap layout and insufficient condensation temperature make it difficult to completely capture all solvent vapors. This can easily lead to some solvents penetrating into the vacuum pump and contaminating the vacuum pump oil, damaging the vacuum pump and causing environmental pollution in the laboratory.

[0005] (2) Samples are easily damaged: Infrared traditional heating methods lead to uneven heating, local overheating causes denaturation and inactivation of bioactive substances or sample boiling, resulting in loss.

[0006] (3) Low degree of automation: The process relies heavily on manual monitoring, which is inefficient and the results of different operators are not repeatable.

[0007] (4) Solvent recovery is difficult: the solvents after condensation are mixed and collected, making it difficult to effectively separate and recycle them.

[0008] Therefore, this invention proposes a multi-stage low-temperature condensation high-vacuum solvent collection system to solve the above problems. Summary of the Invention

[0009] The purpose of this invention is to overcome the above-mentioned shortcomings and provide a multi-stage low-temperature condensation high-vacuum solvent collection system, which is a low-temperature multi-stage condensation high-vacuum concentration system with high collection efficiency, good sample protection and high degree of automation.

[0010] The purpose of this utility model is achieved as follows: A multi-stage cryogenic condensation high-vacuum solvent collection system includes a high-vacuum chamber, a multi-stage gradient cold trap system, a high-vacuum unit, and an intelligent control system. The high-vacuum chamber is connected to the multi-stage gradient cold trap system, the multi-stage gradient cold trap system is connected to the high-vacuum unit, and the high-vacuum chamber, the multi-stage gradient cold trap system, and the high-vacuum unit are respectively connected to the intelligent control system. The high-vacuum chamber is equipped with a multi-layer support for sample containers, and multiple rotating trays are provided on the multi-layer support for sample containers. Material containers are provided on the rotating trays, and each material container is placed on a corresponding rotating tray. Multiple heaters are asymmetrically distributed below the rotating trays. The heaters are connected to an intelligent control system. The intelligent control system controls the rotation frequency of the rotating trays and links it with the microwave heating power of the heaters to achieve dynamic and uniform heating. The multi-stage gradient cold trap system includes at least two stages of cold trap assemblies connected in series. Each stage of the cold trap assembly can independently control its operating temperature. Each stage of the cold trap assembly includes a cold trap of its own, and the operating temperature of each cold trap is arranged in a manner that decreases progressively from the cold trap assembly closer to the high vacuum chamber to the cold trap assembly closer to the high vacuum unit. Each stage of the cold trap is connected to a matching refrigeration unit, and the bottom of each stage of the cold trap is connected to a matching solvent tank. The high vacuum chamber is connected to the cold trap assembly closer to the high vacuum chamber via a high vacuum valve, and the cold trap assembly closer to the high vacuum unit is connected to the high vacuum unit. The intelligent control system is connected to the high vacuum chamber via a first pressure transmitter, a first temperature transmitter, and a nitrogen purging valve; the intelligent control system is connected to each of the aforementioned valve bodies; and the intelligent control system is connected to the high vacuum unit via a second pressure transmitter and a second temperature transmitter.

[0011] Furthermore, the heater is a frequency-controlled magnetic microwave generator.

[0012] Furthermore, the multi-stage gradient cold trap system includes three cold trap assemblies arranged in series. The first-stage cold trap assembly includes a first-stage refrigeration unit, a first-stage cold trap, and a first solvent tank. The second-stage cold trap assembly includes a second-stage refrigeration unit, a second-stage cold trap, and a second solvent tank. The third-stage cold trap assembly includes a third-stage refrigeration unit, a third-stage cold trap, and a third solvent tank.

[0013] Furthermore, the first-stage refrigeration unit is connected to the first-stage cold trap via a first manual valve and a first pneumatic valve. The bottom of the first-stage cold trap is connected to the inlet of the first solvent tank via a stainless steel pipe and a pneumatic valve to collect the liquid solvent after the cold trap condenses. The bottom of the first solvent tank is provided with a first solvent tank drain port. The second-stage refrigeration unit is connected to the second-stage cold trap via a second manual valve and a second pneumatic valve. The bottom of the second-stage cold trap is connected to the inlet of the second solvent tank via a stainless steel pipe and a pneumatic valve to collect the liquid solvent after the cold trap condenses. The bottom of the second solvent tank is provided with a second solvent tank drain port. The third-stage refrigeration unit is connected to the third-stage cold trap via a third manual valve and a third pneumatic valve. The bottom of the third-stage cold trap is connected to the inlet of the third solvent tank via a stainless steel pipe and a pneumatic valve to collect the liquid solvent after the cold trap condenses. The bottom of the third solvent tank is provided with a third solvent tank drain port.

[0014] Furthermore, the high-vacuum cavity is connected to the first-stage cold trap via a high-vacuum valve, the first-stage cold trap is connected to the second-stage cold trap, the second-stage cold trap is connected to the third-stage cold trap, and the third-stage cold trap is connected to the high-vacuum unit.

[0015] Furthermore, the operating temperature range of the first-stage cold trap is -30℃ to -60℃, and the first-stage refrigeration unit is a conventional refrigeration unit; the operating temperature range of the second-stage cold trap is -60℃ to -100℃, and the second-stage refrigeration unit is a cryogenic refrigeration unit; the operating temperature range of the third-stage cold trap is -100℃ to -170℃, and the third-stage refrigeration unit is an ultra-low temperature refrigeration unit or a liquid nitrogen cooling device.

[0016] Furthermore, the surface of the high vacuum chamber is provided with an anti-corrosion layer, and the inner wall of the high vacuum chamber is coated with a Teflon coating or a glass coating.

[0017] Furthermore, the high-vacuum chamber is made of corrosion-resistant medical stainless steel, and the multi-layer support for the sample container inside the high-vacuum chamber is made of corrosion-resistant and low-adsorption material.

[0018] Furthermore, the intelligent control system 4 includes a human-machine interface with a touch screen and a PLC controller. The intelligent control system can preset concentration programs for various biopharmaceutical samples and can monitor, record and provide feedback in real time on key parameters such as material temperature, internal temperature, pressure, cold trap temperature and operation of various freezers and vacuum pumps.

[0019] Furthermore, the high vacuum unit adopts a Roots screw high vacuum pump set, which is a combination of two dry oil-free vacuum pumps connected in series.

[0020] Compared with the prior art, the beneficial effects of this utility model are: This invention provides a multi-stage cryogenic condensation high-vacuum solvent capture system, comprising a high-vacuum chamber, a microwave heating system, a high-vacuum unit, a multi-stage cryogenic condensation capture system, an intelligent control system, and a solvent recovery system. Through a multi-stage gradient cold trap design, combined with microwave heating technology and intelligent control, it achieves highly efficient solvent capture and recovery, significantly improving capture efficiency, protecting sample activity, and enhancing automation. It is suitable for solvent concentration and recovery in fields such as biomedicine, food, and chemicals. It possesses the following specific advantages: (1) Extremely high solvent capture rate: Microwave heating replaces infrared heating, resulting in rapid and uniform heating; Multi-level gradient cold trap design, especially the ultra-low temperature cold trap, can almost completely capture all solvent vapors, protect the vacuum pump, avoid environmental pollution, and facilitate solvent recovery.

[0021] (2) Excellent sample activity protection: The combination of uniform low-temperature heating and high vacuum environment greatly reduces the risk of sample oxidation and denaturation, making it particularly suitable for the concentration of high-value biological samples.

[0022] (3) High degree of automation and reproducibility: The preset program can be started with one click, and no one is needed. This reduces human error and ensures the accuracy and reliability of the experimental results.

[0023] (4) High efficiency and high throughput: The high vacuum chamber can process multiple samples at the same time, and the rotating design improves space utilization and heating efficiency. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the structure of this utility model.

[0025] Figure 2 This is a flowchart illustrating the capture method of this utility model.

[0026] in: 1. High vacuum chamber; 1.1 Material container; 1.2 Rotating tray; 1.3 Heater; 2. Multi-stage gradient cold trap system; 2.1 First-stage refrigeration unit; 2.2 First-stage cold trap; 2.3 First manual valve; 2.4 First pneumatic valve; 2.5 First solvent tank; 2.6 First solvent tank drain port; 2.7 Second-stage refrigeration unit; 2.8 Second-stage cold trap; 2.9 Second manual valve; 2.10 Second pneumatic valve; 2.11 Second solvent tank; 2.12 Second solvent tank. 2.12, third-stage refrigeration unit 2.13, third-stage cold trap 2.14, third manual valve 2.15, third pneumatic valve 2.16, third solvent tank 2.17, third solvent tank drain 2.18, high vacuum unit 3, intelligent control system 4, first pressure transmitter 4.1, first temperature transmitter 4.2, nitrogen venting valve 4.3, high vacuum valve 4.4, second pressure transmitter 4.5, second temperature transmitter 4.6. Detailed Implementation

[0027] To better understand the technical solution of this utility model, a detailed description will be provided below in conjunction with relevant illustrations. It should be understood that the specific embodiments described below are not intended to limit the specific implementation of the technical solution of this utility model, but are merely possible implementations of the technical solution of this utility model. It should be noted that the descriptions of the positional relationships of the components herein, such as component A being located above component B, are based on the relative positions of the components in the illustrations and are not intended to limit the actual positional relationships of the components. Example

[0028] See Figure 1-2 , Figure 1 A schematic diagram of the structure of this utility model has been drawn. As shown in the figure, a multi-stage low-temperature condensation high-vacuum solvent collection system includes a high-vacuum chamber 1, a multi-stage gradient cold trap system 2, a high-vacuum unit 3, and an intelligent control system 4. The high-vacuum chamber 1 is connected to the multi-stage gradient cold trap system 2, the multi-stage gradient cold trap system 2 is connected to the high-vacuum unit 3, and the high-vacuum chamber 1, the multi-stage gradient cold trap system 2, and the high-vacuum unit 3 are respectively connected to the intelligent control system 4.

[0029] The high-vacuum chamber 1 is equipped with a multi-layer support for sample containers. Multiple rotating trays 1.2 are mounted on the multi-layer support, each rotating tray 1.2 being a rotatable circular turntable. Material containers 1.1 are mounted on each rotating tray 1.2, with each material container 1.1 positioned on its corresponding rotating tray 1.2. Below each rotating tray 1.2 are multiple asymmetrically distributed heaters 1.3, each heater 1.3 being a frequency-controlled magnetic microwave generator. Each heater 1.3 is connected to an intelligent control system 4, which controls the rotation frequency of the rotating trays 1.2 in conjunction with the microwave heating power of the heaters 1.3 to achieve dynamic and uniform heating.

[0030] The multi-level gradient cold trap system 2 includes at least two levels of cold trap components arranged in series. Each level of the cold trap component can independently control its operating temperature, and the temperature is arranged in a manner that gradually decreases from the side closer to the high vacuum chamber 1 to the side closer to the high vacuum unit 3.

[0031] In this embodiment, the multi-stage gradient cold trap system 2 includes three cold trap assemblies arranged in series. The first-stage cold trap assembly includes a first-stage refrigeration unit 2.1, a first-stage cold trap 2.2, and a first solvent tank 2.5. The second-stage cold trap assembly includes a second-stage refrigeration unit 2.7, a second-stage cold trap 2.8, and a second solvent tank 2.11. The third-stage cold trap assembly includes a third-stage refrigeration unit 2.13, a third-stage cold trap 2.14, and a third solvent tank 2.17. The first stage refrigeration unit 2.1 is connected to the first stage cold trap 2.2 through the first manual valve 2.3 and the first pneumatic valve 2.4 respectively. The bottom of the first stage cold trap 2.2 is connected to the inlet of the first solvent tank 2.5 through a stainless steel pipe and a pneumatic valve to collect the liquid solvent after the cold trap condenses. The bottom of the first solvent tank 2.5 is provided with a first solvent tank drain port 2.6. The second-stage refrigeration unit 2.7 is connected to the second-stage cold trap 2.8 via the second manual valve 2.9 and the second pneumatic valve 2.10. The bottom of the second-stage cold trap 2.8 is connected to the inlet of the second solvent tank 2.11 via a stainless steel pipe and a pneumatic valve to collect the liquid solvent after the cold trap condenses. The bottom of the second solvent tank 2.11 is provided with a second solvent tank drain port 2.12. The third-stage refrigeration unit 2.13 is connected to the third-stage cold trap 2.14 via a third manual valve 2.15 and a third pneumatic valve 2.16. The bottom of the third-stage cold trap 2.14 is connected to the inlet of the third solvent tank 2.17 via a stainless steel pipe and a pneumatic valve to collect the liquid solvent after the cold trap condenses. The bottom of the third solvent tank 2.17 is provided with a third solvent tank drain port 2.18. The high vacuum chamber 1 is connected to the first-stage cold trap 2.2 via a high vacuum valve 4.4. The first-stage cold trap 2.2 is connected to the second-stage cold trap 2.8. The second-stage cold trap 2.8 is connected to the third-stage cold trap 2.14. The third-stage cold trap 2.14 is connected to the high vacuum unit 3.

[0032] The first-stage cold trap 2.2 operates in a temperature range of -30°C to -60°C, and the first-stage refrigeration unit 2.1 is a conventional refrigeration unit; the second-stage cold trap 2.8 operates in a temperature range of -60°C to -100°C, and the second-stage refrigeration unit 2.7 is a cryogenic refrigeration unit; the third-stage cold trap 2.14 operates in a temperature range of -100°C to -170°C, and the third-stage refrigeration unit 2.13 is an ultra-low temperature refrigeration unit or a liquid nitrogen cooling device.

[0033] The intelligent control system 4 is connected to the high vacuum chamber 1 via a first pressure transmitter 4.1, a first temperature transmitter 4.2, and a nitrogen purging valve 4.3; the intelligent control system 4 is connected to a high vacuum valve 4.4; the intelligent control system 4 is connected to a first pneumatic valve 2.4, a second pneumatic valve 2.10, and a third pneumatic valve 2.16; the intelligent control system 4 is connected to the valves at the inlets and outlets of the first solvent tank 2.5, the second solvent tank 2.11, and the third solvent tank 2.17; the intelligent control system 4 is connected to the high vacuum unit 3 via a second pressure transmitter 4.5 and a second temperature transmitter 4.6.

[0034] In this embodiment, the high vacuum chamber 1 is made of corrosion-resistant medical stainless steel and the surface is treated with anti-corrosion, that is, an anti-corrosion layer is set on the surface of the chamber. The door of the high vacuum chamber 1 is equipped with a transparent glass observation window and a sealing ring.

[0035] In this embodiment, the inner wall of the high vacuum cavity 1 is coated with sanitary Teflon or glass coating.

[0036] In this embodiment, the multi-layer support for the sample container inside the high vacuum chamber 1 is made of a corrosion-resistant and low-adsorption material.

[0037] In this embodiment, the intelligent control system 4 includes a human-machine interface with a touch screen and a PLC controller. The intelligent control system 4 can preset concentration programs for various biomedical samples and can monitor, record and provide feedback in real time on key parameters such as material temperature, internal temperature, pressure, cold trap temperature and operation of various freezers and vacuum pumps.

[0038] In this embodiment, the high vacuum unit 3 adopts a Roots screw high vacuum pump unit, which is a combination of two dry oil-free vacuum pumps connected in series.

[0039] Working principle: This utility model discloses a multi-stage cryogenic condensation high-vacuum solvent collection system, comprising: High vacuum chamber: It is usually made of corrosion-resistant medical stainless steel and its surface is also treated with anti-corrosion. The chamber door is equipped with a transparent glass observation window and a sealing ring; the inside of the chamber is equipped with a rotating sample rack that can hold multiple sample loading containers at the same time.

[0040] Heating system: It adopts non-contact microwave heating technology with asymmetrical heating plates. Combined with the rotation of the sample holder, it can achieve gentle and uniform heating of the sample and avoid local overheating of the drug.

[0041] High vacuum unit: It adopts a Roots screw high vacuum pump unit. The vacuum unit is a combination of two dry oil-free vacuum pumps in series, which is more friendly to the pumped medium. No waste gas or waste liquid is generated. It can achieve and maintain a high vacuum (such as 0.5 Pa) in the vacuum concentration chamber in a short time.

[0042] The cryogenic condensation and capture system employs a multi-stage cold trap series design. The first stage is a conventional refrigeration compressor cold trap with a condensation temperature of -30℃ to -60℃, used to capture most water vapor. The second cryogenic cold trap, achieved through a cryogenic freezer, has a condensation temperature of -60℃ to -100℃. The third stage is an ultra-low temperature cold trap, achieved through an ultra-low temperature freezer, with a condensation temperature of -100℃ to -170℃, specifically designed for the deep capture of non-volatile organic solvent vapors. This multi-stage, gradient cold trap layout significantly improves solvent capture and recovery efficiency, protects the safe operation of the vacuum pump, and greatly reduces energy consumption and saves production costs.

[0043] Intelligent control system: Integrating PLC and touch screen, it can set, store, and recall various concentration programs; the system monitors the concentration process in real time through pressure and temperature sensors, and can automatically adjust heating power, vacuum pump operating frequency, cold trap cooling temperature, etc., to ensure that the concentration process is carried out under optimal parameters. It has functions such as automatic cold trap defrosting and automatic solvent recovery.

[0044] The present invention discloses a method for implementing a multi-stage low-temperature condensation high-vacuum solvent collection system, comprising the following steps: 1. Place the vessel containing the sample solution to be processed on the rotating tray inside the high vacuum chamber; 2. The preset concentration program is initiated through the intelligent control system; 3. Start the vacuum pumps of each stage of the high vacuum unit and evacuate the high vacuum chamber and cryogenic condensation system to the required target vacuum level; 4. Start each stage of the refrigeration unit and open the condensate inlet valve of each stage of the cold trap to cool the multiple cold traps to the set temperature; 5. Start the microwave heating generator and heat the sample solution according to the program; 6. After the solution sample in the high vacuum chamber reaches a certain temperature, the internal solvent begins to evaporate. These solvent vapors enter the multi-stage cold traps in sequence and are condensed and collected stage by stage. The concentration process continues until the end. 7. After evaporation is complete, the system automatically stops heating. The nitrogen venting valve introduces inert gas into the high vacuum chamber to break the vacuum, and the chamber door is opened to remove the concentrated sample.

[0045] The specific operating steps are as follows: The sample solution is dispensed into multiple sample containers (i.e., material containers), and the sample containers are placed on a rotating disk inside a high-vacuum chamber. The door of the high-vacuum chamber is then closed. Select the "Concentrate Aqueous Solution of Sample X" program on the touchscreen; Select the automatic operation process of the system: First, open the pneumatic butterfly valve on the evacuation pipeline, and start the vacuum pumps of each stage of the high vacuum system to pre-evacuate the system; at the same time, start the refrigerant inlet valve of the multi-stage cold trap to cool the first stage cold trap to -60℃, the second stage cold trap to -100℃, and the third stage cold trap to -160℃. When the pressure inside the high vacuum chamber drops to 10 Pa, the microwave heater is activated, and the sample turntable is started to rotate slowly to begin the concentration of the sample. During the concentration process, a large amount of evaporated water vapor is captured by the first-stage cold trap, while a very small amount of escaped water vapor is completely captured by the second-stage cold trap; the evaporated high-saturation-temperature solvent is captured by the second-stage cold trap, and the low-saturation-temperature solvent is captured by the third-stage cold trap. After a certain period of concentration, the system will give a signal that the concentration process is complete once the weight sensor data of the rotating tray reaches the set value. The system will then close the main valve (i.e., the high vacuum valve), automatically stop the heater, and fill the high vacuum chamber with nitrogen to break the vacuum. The system will also stop the refrigeration compressor, close the refrigerant valve, and stop all stages of the vacuum pumps in the high vacuum unit.

[0046] In the research and development and production of biopharmaceutical products, such as proteins, peptides, vaccines, and nucleic acid drugs, a large amount of volatile organic solvents (such as methanol, ethanol, ethylene glycol, acetone, dichloromethane, etc.) are often used in the freeze-drying, solvent replacement, concentration, and post-processing of chemical polymerization reactions. These processes must be carried out in a low-temperature, vacuum environment to lower the boiling point of the materials and avoid the inactivation and contamination of heat-sensitive substances.

[0047] This invention discloses a multi-stage low-temperature solvent condensation and trapping high-vacuum device for biopharmaceutical products. The device employs a multi-stage temperature gradient cold trap design, combined with high-vacuum technology and a cascade refrigeration system, enabling efficient recovery of various organic solvents used in biopharmaceutical production. This invention achieves separation of solvents with different boiling points through staged condensation, achieving a recovery purity of over 99%, significantly reducing production costs and environmental pollution.

[0048] The innovative points of this utility model are: (1) Multi-level gradient cold trap design: The temperature of the three-level cold trap is gradually reduced to achieve efficient capture and separation of solvents with different boiling points.

[0049] (2) Combining microwave heating with rotating sample holder: to achieve uniform heating of the sample and avoid local overheating.

[0050] (3) Intelligent control system: realizes full-process automated control, improves operation convenience and result reproducibility.

[0051] Main application areas of this utility model: Concentrated fruit juices (orange juice, apple juice), vegetable juices, milk, honey, seasonings (soy sauce, vinegar), flavorings, and extracts of traditional Chinese medicine in the food industry are used to maintain their natural flavor and nutrition. In the pharmaceutical industry, concentrated traditional Chinese medicine extracts, antibiotics, vitamins, enzyme preparations, vaccines, and other heat-sensitive biological products are used to ensure drug activity. Concentrated proteins, nucleic acids, cell culture media, fermentation broths, etc., used in the bioengineering industry; In the chemical industry, applications include the recovery of organic solvents, the concentration of fine chemicals, and the treatment of high-salt wastewater.

[0052] The above are merely specific application examples of this utility model and do not constitute any limitation on the scope of protection of this utility model. All technical solutions formed by equivalent transformations or equivalent substitutions fall within the scope of protection of this utility model.

Claims

1. A multi-stage cryogenic condensation high-vacuum solvent collection system, characterized in that: It includes a high vacuum chamber (1), a multi-stage gradient cold trap system (2), a high vacuum unit (3), and an intelligent control system (4). The high vacuum chamber (1) is connected to the multi-stage gradient cold trap system (2), the multi-stage gradient cold trap system (2) is connected to the high vacuum unit (3), and the high vacuum chamber (1), the multi-stage gradient cold trap system (2), and the high vacuum unit (3) are respectively connected to the intelligent control system (4). The high vacuum chamber (1) is equipped with a multi-layer support for sample containers. The multi-layer support for sample containers is equipped with multiple rotating trays (1.2). The rotating trays (1.2) are equipped with material containers (1.1). Each material container (1.1) is set on a corresponding rotating tray (1.2). Below the rotating trays (1.2) are multiple heaters (1.3) that are asymmetrically distributed. The heaters (1.3) are respectively connected to the intelligent control system (4). The intelligent control system (4) controls the rotation frequency of the rotating trays (1.2) and the microwave heating power of the heaters (1.3) to achieve dynamic and uniform heating. The multi-stage gradient cold trap system (2) includes at least two stages of cold trap components arranged in series. The operating temperature of each stage of the cold trap component can be independently controlled. Each stage of the cold trap component includes a stage of cold traps. The operating temperature of each stage of the cold trap is arranged in a manner that gradually decreases from the cold trap component near the high vacuum chamber (1) to the cold trap component near the high vacuum unit (3). Each stage of the cold trap is connected to a matching refrigeration unit, and the bottom of each stage of the cold trap is connected to a matching solvent tank. The high vacuum chamber (1) is connected to the cold trap component near the high vacuum chamber (1) through a high vacuum valve (4.4), and the cold trap component near the high vacuum unit (3) is connected to the high vacuum unit (3). The intelligent control system (4) is connected to the high vacuum chamber (1) through the first pressure transmitter (4.1), the first temperature transmitter (4.2) and the purging nitrogen valve (4.3); the intelligent control system (4) is connected to each of the above valve bodies; the intelligent control system (4) is connected to the high vacuum unit (3) through the second pressure transmitter (4.5) and the second temperature transmitter (4.6).

2. The multi-stage cryogenic condensation high-vacuum solvent collection system according to claim 1, characterized in that: The heater (1.3) is a frequency-controlled magnetic microwave generator.

3. The multi-stage cryogenic condensation high-vacuum solvent collection system according to claim 1, characterized in that: The multi-stage gradient cold trap system (2) includes three cold trap components arranged in series. The first-stage cold trap component includes a first-stage refrigeration unit (2.1), a first-stage cold trap (2.2), and a first solvent tank (2.5). The second-stage cold trap component includes a second-stage refrigeration unit (2.7), a second-stage cold trap (2.8), and a second solvent tank (2.11). The third-stage cold trap component includes a third-stage refrigeration unit (2.13), a third-stage cold trap (2.14), and a third solvent tank (2.17).

4. The multi-stage cryogenic condensation high-vacuum solvent collection system according to claim 3, characterized in that: The first stage refrigeration unit (2.1) is connected to the first stage cold trap (2.2) through the first manual valve (2.3) and the first pneumatic valve (2.4). The bottom of the first stage cold trap (2.2) is connected to the inlet of the first solvent tank (2.5) through a stainless steel pipe and a pneumatic valve to collect the liquid solvent after the cold trap condenses. The bottom of the first solvent tank (2.5) is provided with a first solvent tank drain port (2.6). The second-stage refrigeration unit (2.7) is connected to the second-stage cold trap (2.8) via a second manual valve (2.9) and a second pneumatic valve (2.10). The bottom of the second-stage cold trap (2.8) is connected to the inlet of the second solvent tank (2.11) via a stainless steel pipe and a pneumatic valve to collect the liquid solvent after the cold trap condenses. The bottom of the second solvent tank (2.11) is provided with a second solvent tank drain port (2.12). The third-stage refrigeration unit (2.13) is connected to the third-stage cold trap (2.14) via a third manual valve (2.15) and a third pneumatic valve (2.16). The bottom of the third-stage cold trap (2.14) is connected to the inlet of the third solvent tank (2.17) via a stainless steel pipe and a pneumatic valve to collect the liquid solvent after the cold trap condenses. The bottom of the third solvent tank (2.17) is provided with a third solvent tank drain port (2.18).

5. The multi-stage cryogenic condensation high-vacuum solvent collection system according to claim 3, characterized in that: The high vacuum chamber (1) is connected to the first-stage cold trap (2.2) via a high vacuum valve (4.4), the first-stage cold trap (2.2) is connected to the second-stage cold trap (2.8), the second-stage cold trap (2.8) is connected to the third-stage cold trap (2.14), and the third-stage cold trap (2.14) is connected to the high vacuum unit (3).

6. The multi-stage cryogenic condensation high-vacuum solvent collection system according to claim 3, characterized in that: The operating temperature range of the first-stage cold trap (2.2) is -30°C to -60°C, the operating temperature range of the second-stage cold trap (2.8) is -60°C to -100°C, and the operating temperature range of the third-stage cold trap (2.14) is -100°C to -170°C.

7. The multi-stage cryogenic condensation high-vacuum solvent collection system according to claim 1, characterized in that: The surface of the high vacuum chamber (1) is provided with an anti-corrosion layer, and the inner wall of the high vacuum chamber (1) is coated with a Teflon coating or a glass coating.

8. The multi-stage cryogenic condensation high-vacuum solvent collection system according to claim 1, characterized in that: The high vacuum chamber (1) is made of corrosion-resistant medical stainless steel, and the multi-layer support of the sample container inside the high vacuum chamber (1) is made of corrosion-resistant and low-adsorption material.

9. The multi-stage cryogenic condensation high-vacuum solvent collection system according to claim 1, characterized in that: The intelligent control system (4) includes a human-machine interface with a touch screen and a PLC controller. The intelligent control system (4) can preset a variety of biomedical sample concentration programs and can monitor, record and provide feedback on key parameters such as material temperature, internal temperature, pressure, cold trap temperature and operation of various freezers and vacuum pumps in real time.

10. A multi-stage cryogenic condensation high-vacuum solvent collection system according to claim 1, characterized in that: The high vacuum unit (3) adopts a Roots screw high vacuum pump unit, which is a combination of two dry oil-free vacuum pumps connected in series.

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