Integrated degassing and uniform mixing device and system and use method of integrated degassing and uniform mixing device and system
By integrating vacuum degassing and vortex mixing functions, the problem of poor handling of thermosensitive samples by vacuum degassing and the difficulty in overcoming interfacial tension in vortex mixers has been solved, achieving efficient homogenization of complex samples and improving the accuracy of experimental results.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-17
- Publication Date
- 2026-04-03
AI Technical Summary
In existing technologies, vacuum degassing devices are not effective for processing thermosensitive samples, and vortex mixers are unable to overcome interfacial tension in multiphase systems and cannot effectively break up micron-sized bubbles, resulting in inaccurate experimental results and cumbersome operation.
An integrated degassing and homogenizing device was designed, which integrates vacuum degassing and vortex homogenizing functions. Through the combination of vertical and horizontal design, a negative pressure environment is established by the vacuum unit and combined with the vortex motion of the rotation drive unit to achieve efficient homogenization of complex samples.
It improves the accuracy and repeatability of experimental results, shortens the degassing cycle, reduces operating steps, lowers equipment maintenance costs, and is suitable for various laboratory scenarios.
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Figure CN121783665A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of detection technology, and in particular to an integrated degassing and mixing device, system, and method of use thereof. Background Technology
[0002] In laboratory sample preparation and analysis, especially in high-performance liquid chromatography (HPLC) and ion chromatography systems, the performance analysis of various solutions is involved. On the one hand, dissolved gases in the solution can disrupt the stability of the mobile phase, leading to problems such as baseline drift. On the other hand, in physical property analyses such as specific gravity determination, residual bubbles can interfere with measurement accuracy. Therefore, removing dissolved gases from the solution is crucial to ensuring the accuracy of test results.
[0003] Current methods for degassing solutions include ultrasound, vacuum treatment, freezing, bubbling, helium degassing, and vortexing. Among these, ultrasound degassing can damage heat-sensitive materials, freezing is time-consuming and unsuitable for samples sensitive to ice crystals, bubbling is limited for high-boiling-point solvents, and helium degassing is costly. Therefore, vacuum degassing has become the mainstream technique due to its ease of operation and lack of reagent requirements; it can promote the escape of dissolved gases by reducing gas pressure. Vortex mixing degassing utilizes the centrifugal and shear forces generated by high-speed circular motion to break up bubbles while mixing the sample; it is also widely used for its high efficiency in degassing low-viscosity solutions.
[0004] However, both have significant drawbacks when used individually: vacuum degassing devices are ineffective for processing heat-sensitive samples and require cumbersome repeated cycles; traditional vortex mixers, with their unidirectional vortex mode, struggle to overcome interfacial tensions in multiphase systems, and the lack of vacuum coordination leads to easy splashing of trace samples and an inability to effectively break up micron-sized bubbles. Therefore, an integrated device combining vacuum degassing and vortex mixing functions has become a research hotspot. Summary of the Invention
[0005] The purpose of this invention is to provide an integrated device, system, and method of using that integrates vacuum degassing and vortex mixing functions.
[0006] To achieve the above objectives, this application employs the following technical solution: On the one hand, this application provides an integrated degassing and mixing device, including... A container stage, at least for supporting a sample container, is disposed on a first working surface, the sample container being used to hold a sample to be degassed; A sealing unit, at least for sealing the opening of the sample container, so that the inner cavity of the sample container is formed as a closed cavity; A lifting drive unit is connected to the sealing unit and is at least used to drive the sealing unit to move along the second working surface between the first working position and the second working position. At the first working position, the sealing unit seals the opening of the sample container, and at the second working position, the sealing unit moves away from the opening of the sample container. The second working surface is perpendicular to the first working surface. A rotary drive unit, connected to the sample container, is used at least to drive the sample container sealed by the sealing unit to rotate; A vacuum unit, connected to the enclosed cavity, is used at least to establish and maintain a negative pressure environment within the enclosed cavity.
[0007] As a further improvement of this application, a horizontal drive unit is also included, the horizontal drive unit including a guide rail and a drive mechanism, the guide rail extending along the first working surface, the container platform being movably disposed on the guide rail, and the drive mechanism being used to drive the container platform to approach or move away from the first work station along the guide rail.
[0008] As a further improvement to this application, the driving mechanism is a servo motor or a stepper motor.
[0009] As a further improvement of this application, the sealing unit is provided with a through hole, and the vacuum unit communicates with the closed cavity through the through hole.
[0010] As a further improvement of this application, the device also includes a high-speed rotary joint disposed on the through hole, and the vacuum unit is connected to the sealing unit through the high-speed rotary joint.
[0011] As a further improvement of this application, the device also includes a clamping unit located on the second working surface and below the sealing unit for clamping or releasing the sample container.
[0012] As a further improvement of this application, the clamping unit is provided with a pressure sensor for real-time feedback of the clamping status of the clamping unit.
[0013] As a further improvement of this application, the container stage is equipped with a rotatable cylindrical structure including a bottom bearing. The cylinder of the rotatable cylindrical structure has a built-in slot design for adapting to the sample container, and the bottom bearing is used to provide support for the sample container.
[0014] On the other hand, this application also provides an integrated degassing and mixing system, including the integrated degassing and mixing device described in any one of the first aspects, a first workbench and a second workbench; wherein the container platform and the lifting drive unit are respectively disposed on the first workbench and the second workbench.
[0015] In another aspect, this application also provides a method for using an integrated degassing and mixing system, comprising the following steps: S1. Place the sample container of the sample to be degassed on the container platform of the first workbench; S2. The horizontally driven container stage moves along the first worktable to the preset working position directly below the sealing unit; S3. The sealing unit and the rotary drive unit located on the second worktable are driven to descend vertically, so that the sealing unit and the sample container are sealed to form a closed cavity. S4. Start the vacuum unit to evacuate the sealed cavity through the sealing unit to establish and maintain a negative pressure environment; start the rotary drive unit to drive the sealing unit and sample container to rotate, so that the sample to be degassed in the sample container forms a vortex and achieves uniform mixing, and the rotary drive unit periodically switches the direction according to the preset program. S5. Shut down the vacuum unit to break the negative pressure environment inside the sealed cavity; S6. The sealing unit and the rotary drive unit are driven to rise vertically by the lifting drive unit, so that the sealing unit is separated from the sample container. S7. The horizontally driven container stage moves along the first worktable to the initial position to remove the processed sample container.
[0016] The specific benefits of this application are as follows: The horizontal first worktable supports the container platform and sample container, while the vertical second worktable houses the lifting drive unit. This combined vertical and horizontal design ensures a compact layout of all components, significantly reducing the equipment size. Compared to traditional split-type equipment, its size is more suitable for laboratory or automated production line spaces. It also facilitates docking with automated mechanisms such as robotic arms, reducing reliance on manual labor. The container platform stably supports the sample container, ensuring precise container positioning during subsequent operations and providing a foundation for sealing and rotation. The sealing unit, located above the sample container, works in conjunction with the vertical reciprocating motion of the lifting drive unit to quickly seal or open the sample container. This convenient operation and highly reliable sealing avoid the cumbersome manual operation and secondary contamination risks associated with traditional open sample chambers. The rotary drive unit is connected to the sealing unit, enabling the sealing unit and sample container to rotate. Combined with the negative pressure environment (e.g., -70 kPa) established by the vacuum unit within the closed cavity, it overcomes the limitations of traditional vacuum degassing, which relies solely on negative pressure and vortex mixing in a single direction. By utilizing vacuum to reduce interfacial tension and gas resistance, it enhances the dispersion effect of vortex shear force on heterogeneous substances, achieving efficient homogenization of complex samples. The negative pressure environment reduces the solubility of gases in the liquid, promoting gas escape. Simultaneously, the centrifugal force and shear force generated by rotation form vortices, which not only accelerate the migration of bubbles to the liquid surface to improve degassing efficiency, shorten the degassing cycle, and reduce repeated degassing operations, but also thoroughly mixes complex samples with large density differences and multiphase stratification, eliminating mixing dead zones and solving the process redundancy problems caused by traditional step-by-step operations. In addition, the overall structure has no complex mechanical transmission contact parts (such as gears, belts, etc.), which reduces wear, extends equipment life, and reduces maintenance costs. The vacuum unit can stably maintain negative pressure, and with the adjustable speed characteristics of the rotary drive, it can adapt to samples of different viscosities and types, taking into account both thorough degassing and uniform mixing, improving the accuracy and repeatability of experimental results. It is suitable for various laboratory scenarios such as ion chromatography eluent treatment and brine density detection. Attached Figure Description
[0017] Figure 1 This is a schematic diagram of the integrated degassing and mixing device in the example of this application.
[0018] In the figure: 1. First worktable; 2. Second worktable; 3. Container stage; 4. Sample container; 5. Sealing unit; 6. Rotary drive unit; 7. High-speed rotary joint; 8. Lifting cylinder; 9. Cylinder solenoid valve; 10. Vacuum regulating valve; 11. Vacuum pressure gauge; 12. Vacuum solenoid valve; 13. Clamping unit. Detailed Implementation
[0019] The technical solution of this application will be clearly and completely described below with reference to the embodiments of this application. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of this application. In the three-dimensional coordinate system involved in the drawings, the direction of the Y-axis corresponds to the extension direction of the first working surface in this embodiment.
[0020] To make the above-mentioned objectives, features and advantages of this application more apparent and understandable, the application will be further described in detail below with reference to specific embodiments.
[0021] This application provides an integrated degassing and mixing system, including an integrated degassing and mixing device, a first worktable, and a second worktable; wherein a container platform and a lifting drive unit are respectively disposed on the first worktable and the second worktable.
[0022] The integrated degassing and mixing device includes: A container stage, at least for supporting a sample container, is disposed on a first working surface, the sample container being used to hold a sample to be degassed; A sealing unit, at least for sealing the opening of the sample container, so that the inner cavity of the sample container is formed as a closed cavity; A lifting drive unit is connected to the sealing unit and is at least used to drive the sealing unit to move along the second working surface between the first working position and the second working position. At the first working position, the sealing unit seals the opening of the sample container, and at the second working position, the sealing unit moves away from the opening of the sample container. The second working surface is perpendicular to the first working surface. A rotary drive unit, connected to the sample container, is used at least to drive the sample container sealed by the sealing unit to rotate; A vacuum unit, connected to the enclosed cavity, is used at least to establish and maintain a negative pressure environment within the enclosed cavity.
[0023] Based on the above technical solution, the horizontal first worktable supports the container platform and sample container, while the vertical second worktable houses the lifting drive unit. This combined vertical and horizontal design ensures a compact layout of all components, significantly reducing the equipment size. Compared to traditional split-type equipment, its size is more suitable for laboratory or automated production line spaces. It also facilitates docking with automated mechanisms such as robotic arms, reducing reliance on manual labor. The container platform stably supports the sample container, ensuring precise container positioning during subsequent operations and providing a foundation for sealing and rotation. The sealing unit, located above the sample container, works in conjunction with the vertical reciprocating motion of the lifting drive unit to quickly seal or open the sample container. This convenient operation and highly reliable sealing avoid the cumbersome manual operation and secondary contamination risks associated with traditional open sample chambers. The rotary drive unit is connected to the sealing unit, enabling the sealing unit and sample container to rotate. Combined with the negative pressure environment (e.g., -70 kPa) established by the vacuum unit within the closed cavity, it overcomes the limitations of traditional vacuum degassing, which relies solely on negative pressure and vortex mixing in a single direction. By utilizing vacuum to reduce interfacial tension and gas resistance, it enhances the dispersion effect of vortex shear force on heterogeneous substances, achieving efficient homogenization of complex samples. The negative pressure environment reduces the solubility of gases in the liquid, promoting gas escape. Simultaneously, the centrifugal force and shear force generated by rotation form vortices, which not only accelerate the migration of bubbles to the liquid surface to improve degassing efficiency, shorten the degassing cycle, and reduce repeated degassing operations, but also thoroughly mixes complex samples with large density differences and multiphase stratification, eliminating mixing dead zones and solving the process redundancy problems caused by traditional step-by-step operations. In addition, the overall structure has no complex mechanical transmission contact parts (such as gears, belts, etc.), which reduces wear, extends equipment life, and reduces maintenance costs. The vacuum unit can stably maintain negative pressure, and with the adjustable speed characteristics of the rotary drive, it can adapt to samples of different viscosities and types, taking into account both thorough degassing and uniform mixing, improving the accuracy and repeatability of experimental results. It is suitable for various laboratory scenarios such as ion chromatography eluent treatment and brine density detection.
[0024] In an optional implementation, the integrated degassing and mixing device further includes a horizontal drive unit, which includes a guide rail and a drive mechanism. The guide rail extends along the first working surface, and the container platform is movably mounted on the guide rail. The drive mechanism is used to drive the container platform along the guide rail to approach or move away from the first working station. Preferably, the drive mechanism is a servo motor or a stepper motor.
[0025] Based on the above technical solution, the horizontal drive unit can drive the container stage to reciprocate between the first and second workstations along the guide rail, allowing the container stage to be moved to a position away from or close to the core components such as the sealing unit and the rotary drive unit. This facilitates the safe and efficient loading and unloading of sample containers by manual labor or robotic arms, avoiding the risk of collisions that may occur when operating in the core working area of the equipment. At the same time, it meets the needs of continuous sample feeding by conveyor belts and precise grasping by robotic arms in automated production lines, reducing manual intervention steps and improving the overall automation level of the process.
[0026] Meanwhile, in terms of positioning accuracy and operational stability, the guide rail provides precise motion guidance for the container stage. Combined with the programmed control of the drive mechanism (such as a servo motor or stepper motor), it can ensure that the container stage moves the sample container precisely to the preset working position directly below the sealing unit. The positioning accuracy can meet the requirements of efficient sealing between the sealing unit and the sample container, avoiding problems such as poor sealing and vacuum leakage caused by container position deviation, and ensuring the stability of the subsequent vacuum degassing and vortex mixing process.
[0027] In terms of equipment compatibility and space utilization, this horizontal drive structure can flexibly adjust the movement stroke of the container stage to adapt to the picking, placing and positioning needs of sample containers of different specifications. Moreover, the integrated design of the guide rail and drive mechanism will not significantly increase the space occupied by the first worktable. Combined with the overall vertical and horizontal layout of the device, the spatial structure of the equipment is further optimized, making the equipment more suitable for compact laboratory benchtops or multi-equipment collaborative layouts in automated production lines. At the same time, it provides a structural foundation for possible subsequent multi-station expansion (such as multiple container stages working alternately), which helps to improve the batch processing capacity and work efficiency of the equipment.
[0028] In an optional implementation, the sealing unit has a through hole, through which the vacuum unit communicates with the sealed cavity. The device also includes a high-speed rotary joint disposed on the through hole, through which the vacuum unit connects to the sealing unit. Providing a through hole in the sealing unit for the vacuum unit to communicate with the sealed cavity, and connecting the two with a high-speed rotary joint, achieves several key benefits: Firstly, the high-speed rotary joint maintains the sealed connection of the pipeline to the vacuum unit while the sealing unit rotates at high speed with the rotary drive unit, preventing vacuum leakage during rotation and ensuring a stable negative pressure environment within the sealed cavity (e.g., maintaining a set value of -70 kPa), thus guaranteeing degassing efficiency. Secondly, this design eliminates the problems of pipeline entanglement and pulling caused by the rotation of the sealing unit, reducing pipeline wear and failure risks, and extending equipment lifespan. Simultaneously, it eliminates the need for additional sealing channels to accommodate rotation, simplifying the sealing unit structure, reducing the probability of seal failure, and further improving the overall stability and reliability of the device, adapting to the requirements of continuous vacuum degassing and vortex mixing synchronous operation.
[0029] In an optional implementation, the device further includes a clamping unit located on the second worktable and below the sealing unit, for clamping or releasing the sample container. The clamping unit in this technical solution functions as follows: firstly, during vacuum degassing and vortex mixing operations, it clamps the sample container to prevent displacement or shaking due to the high-speed rotation driven by the rotary drive unit or the negative pressure environment, thus avoiding droplet splashing or adhesion to the container wall and ensuring operational stability; secondly, during vacuum release and the resetting of the sealing unit, it maintains the fixed position of the sample container, providing a stable foundation for the subsequent Y-axis drive mechanism to return the container platform to the pick-up / placement position and complete sample unloading, while also adapting to automated operation processes and reducing manual intervention.
[0030] In an optional implementation, the clamping unit is equipped with a pressure sensor to provide real-time feedback on the clamping status of the clamping unit. The pressure sensor can monitor the clamping force of the clamping unit on the sample container in real time, providing feedback on whether it is clamped too tightly (to prevent loosening that could lead to rotational displacement or droplet splashing) or over-clamped (to prevent damage to the container / affecting the seal), ensuring that the clamping status is adapted to the container specifications and operational requirements, guaranteeing stable vacuum degassing and vortex mixing, and also providing accurate force signals for automated control.
[0031] In an optional implementation, the lifting drive unit includes a lifting cylinder, a cylinder solenoid valve, and an air source; the clamping unit is a pneumatic clamping unit; and the vacuum unit includes a vacuum regulating valve, a vacuum pressure gauge, a vacuum solenoid valve, and a vacuum pump.
[0032] Among them, the vacuum pump can adopt a miniaturized vacuum generation module (such as a vortex dry pump) and a standardized mechanical interface, which reduces the size of the equipment to 1 / 5 of the traditional solution and can be directly embedded into the automated production line to realize continuous batch sample processing.
[0033] In an optional implementation, the container stage is equipped with a rotatable cylindrical structure including a bottom bearing. The cylinder of the rotatable cylindrical structure has a built-in slot design for accommodating the sample container, and the bottom bearing provides support for the sample container. Overall, the structure adopts a design that combines a top non-contact magnetic drive unit with a bottom low-friction bearing for support. Rotation is driven from the top of the container through magnetic coupling, with only a bearing for limiting the bottom. This eliminates leakage caused by openings in the vacuum chamber (maintaining stable vacuum) and compresses the axial space of the equipment by more than 40%, making it suitable for integration into the end effector of robotic arms in automated production lines.
[0034] On the other hand, this application also provides an integrated degassing and mixing device, the specific embodiments of which are consistent with the embodiments described above and the technical effects achieved are the same, and some contents will not be repeated. The integrated degassing and mixing device includes: A container stage, at least for supporting a sample container, is disposed on a first working surface, the sample container being used to hold a sample to be degassed; A sealing unit, at least for sealing the opening of the sample container, so that the inner cavity of the sample container is formed as a closed cavity; A lifting drive unit is connected to the sealing unit and is at least used to drive the sealing unit to move along the second working surface between the first working position and the second working position. At the first working position, the sealing unit seals the opening of the sample container, and at the second working position, the sealing unit moves away from the opening of the sample container. The second working surface is perpendicular to the first working surface. A rotary drive unit, connected to the sample container, is used at least to drive the sample container sealed by the sealing unit to rotate; A vacuum unit, connected to the enclosed cavity, is used at least to establish and maintain a negative pressure environment within the enclosed cavity.
[0035] In another aspect, this application also provides a method for using an integrated degassing and mixing system, comprising the following steps: S1. Place the sample container of the sample to be degassed on the container platform of the first workbench; S2. The horizontally driven container stage moves along the first worktable to the preset working position directly below the sealing unit; S3. The sealing unit and the rotary drive unit located on the second worktable are driven to descend vertically, so that the sealing unit and the sample container are sealed to form a closed cavity. S4. Start the vacuum unit to evacuate the sealed cavity through the sealing unit to establish and maintain a negative pressure environment; start the rotary drive unit to drive the sealing unit and sample container to rotate, so that the sample to be degassed in the sample container forms a vortex and achieves uniform mixing, and the rotary drive unit periodically switches the direction according to the preset program. S5. Shut down the vacuum unit to break the negative pressure environment inside the sealed cavity; S6. The sealing unit and the rotary drive unit are driven to rise vertically by the lifting drive unit, so that the sealing unit is separated from the sample container. S7. The horizontally driven container stage moves along the first worktable to the initial position to remove the processed sample container.
[0036] In a specific example, such as Figure 1As shown, this application provides an integrated degassing and mixing device, including a first workbench 1 located in the horizontal direction and a second workbench 2 perpendicular to the first workbench 1; it also includes a container stage 3, a sample container 4, a sealing unit 5, a rotary drive unit 6, a lifting drive unit, a vacuum unit, and a clamping unit 13, wherein: the container stage 3 is located on the first workbench 1, and the first workbench 1 is provided with a horizontal drive unit including a guide rail and a drive mechanism, the guide rail extends along the first working surface, the container stage is movably disposed on the guide rail, the drive mechanism is used to drive the container stage to approach or move away from the first work position along the guide rail, the drive mechanism is a servo motor or a stepper motor, supports programmed path setting, the container stage 3 is slidably mounted on the guide rail, the output end of the drive mechanism is connected to the container stage 3 to drive the container stage 3 to reciprocate along the extension direction of the guide rail, so as to realize the precise positioning and transmission of the sample container 4, and the container stage 3 is equipped with a bottom bearing ( Figure 1 A rotatable cylindrical structure (not shown) with an internal slot design to accommodate a fixed-size sample container 4. A bottom bearing provides support for the sample container. The sample container 4, located on the container stage 3, is made of PP material and has a capacity range of 1-125mL. It is used to hold samples to be degassed, and its top has a pre-drilled interface for mating with the sealing unit 5. The sealing unit 5 is an integrated rotary sealing plate located above the sample container 4. The surface of the sealing plate is covered with a silicone sealing ring, and the sealing unit 5 has a through hole on which a high-speed rotary joint 7 is installed. This high-speed rotary joint 7 supports continuous sealed transmission of the vacuum unit's tubing during rotation, with a maximum speed compatible with 5000rpm and a leakage rate <1×10⁻⁶. -9 mbar The vacuum unit, operating at L / s, is connected to the sealing unit 5 via a high-speed rotary joint 7 and communicates with the closed cavity. It is used to establish and maintain a negative pressure environment of -70 kPa within the closed cavity. The rotary drive unit 6 is a brushless DC motor with a power of 200W, equipped with an encoder for closed-loop speed control. It is connected to the sealing unit 5 via a synchronous belt, driving the sealing unit 5 and sample container 4 to rotate at speeds of 0~1000 rpm, supporting centrifugation, stirring, and other operations. The lifting drive unit, located on the second worktable 2, includes a lifting cylinder 8, a cylinder solenoid valve 9, and an air source. The lifting cylinder 8 drives the sealing unit 5 and the rotary drive unit 6 to reciprocate vertically, with a stroke range of 0~200 mm and an accuracy of ±0.1 mm. The cylinder solenoid valve 9 is a three-position five-way valve with integrated pressure regulation (0.1~0.8 MPa), supporting multi-cylinder collaborative timing programming to achieve single-cylinder sealing... The sealing and opening of the sample container 4 and the sealing unit 5; the clamping unit 13 is a pneumatic fixed clamping unit 13, located on the second worktable 2 and below the sealing unit 5, driven by a double-acting cylinder, and realizes the rapid clamping and release of the sample container 4 through symmetrical opening and closing claws. The clamping force is adjustable (0~50N). It is equipped with a pressure sensor to provide real-time feedback on the clamping status and prevent overload or slippage. The lifting cylinder 8 and the pneumatic clamping unit 13 are connected to the air source through a three-position five-way valve; the vacuum unit includes a vacuum regulating valve 10, a vacuum pressure gauge 11, a vacuum solenoid valve 12 and a vacuum pump. The vacuum regulating valve 10 is a proportional valve, which controls the vacuum degree with an accuracy of ±0.5kPa. The vacuum pressure gauge 11 is a digital display type with a range of -100kPa to 0kPa and a resolution of 0.1kPa. The vacuum solenoid valve 12 controls the vacuum pipeline with a response time of <50ms and supports automatic or manual mode switching.
[0037] The rotary drive unit here is a brushless DC motor with a speed of 0-1000 rpm and periodically switching directions according to a preset program. This can be understood as achieving bidirectional alternating vortex motion, creating a negative pressure environment (-70 kPa) within the vacuum chamber. Combined with the bidirectional alternating vortex motion, centrifugal force forces bubbles to migrate towards the liquid surface and removes them through negative pressure. Simultaneously, the vortex shear force breaks up micron-sized bubbles and enhances the diffusion of heterogeneous substances, thereby simultaneously achieving high degassing rate and high mixing uniformity. The vortex intensity and vacuum level can be dynamically adjusted through an intelligent feedback system. Under the synergistic effect of negative pressure suppressing solvent evaporation, droplet splashing caused by high-speed rotation is avoided. Ultimately, this achieves a comprehensive technical effect of integrated degassing and mixing processes, significantly reduced energy consumption, and greatly reduced manual intervention.
[0038] In another specific example, the initial state of the integrated degassing and mixing device is as follows: the gas source is connected to the cylinder solenoid valve 9, the gas pressure is adjusted to the set value, the target vacuum degree is set to -70kPa through the vacuum regulating valve 10, and the gas is output in two paths through the vacuum solenoid valve 12. One path is connected to the vacuum pressure gauge 11 to monitor the pressure state in the closed cavity in real time, and the other path is connected to the high-speed rotary joint 7 to provide vacuum adsorption capacity for the sealing plate. The vacuum solenoid valve 12 is initially closed to cut off the passage between the vacuum pump and the closed cavity; the container stage 3 moves to the preset "pick-up and drop-off position". The container stage 3 is in a safe operating area for the user. The clamping unit 13 is fully open, with an opening and closing distance greater than or equal to the diameter of the sample container 4 and an error of ±5mm. No clamping force is applied. The piston rod of the lifting cylinder 8 is fully retracted, driving the sealing pressure plate and the rotary drive unit 6 to a high position, without contact with the sample container 4. The vacuum regulating valve 10 is in manual / standby mode, and the automatic pressure regulation function is not activated. All control circuits of the cylinder solenoid valve 9 are de-energized, the power supply to the rotary motor is disconnected, and the rotor is locked. The device switches to the "initialization complete" state, and the operation interface displays "Ready for Loading". The vacuum pressure gauge 11 reads atmospheric pressure, the pressure sensor feeds back a "not clamped" signal, and the lifting cylinder 8 is confirmed to be in a "high position" state, ensuring that the device is ready to receive operation commands in a safe mode with no load and no power output.
[0039] The workflow of the integrated degassing and mixing system described above is as follows: First, the sample container 4 containing the sample to be degassed is placed in the slot of the container stage 3 by an external mechanism or manually. The horizontal drive unit is activated, moving the container stage 3 along the Y-axis extension direction to the preset working position directly below the sealing plate, with a positioning accuracy of ≤0.5mm. Then, the lifting cylinder 8 extends, pushing the sealing plate vertically downward, so that its silicone sealing ring is tightly fitted with the upper edge of the sample container 4 to form a closed cavity. The vacuum solenoid valve 12 is opened, and the vacuum pump evacuates the closed cavity. The negative pressure gas source enters the sample container 4 through the vacuum regulating valve 10 and the high-speed rotary joint 7, and the vacuum is continuously evacuated to -70kPa (monitored by the vacuum pressure gauge 11), completing the degassing for 10s–60s. Then, the rotary motor is activated. The process involves a synchronous belt driving the sealing plate and sample container 4 to rotate at a set speed. Under centrifugal force, the sample to be degassed inside the sample container 4 forms a high-intensity vortex, achieving uniform mixing. The rotating motor periodically switches directions according to a preset program (e.g., 10 seconds forward rotation → 1 second stop → 10 seconds reverse rotation), changing the vortex direction to enhance the mixing effect, repeating this cycle 3-5 times. Afterward, the vacuum solenoid valve 12 closes to cut off the negative pressure gas source, while atmospheric pressure gas is introduced to disrupt the vacuum environment inside the sample container 4. The clamping unit 13 closes to clamp the sample container 4 to prevent displacement, and the lifting cylinder 8 retracts, causing the sealing plate to rise to its initial high position. Finally, the horizontal drive unit drives the container stage 3 back to the preset "pick-up and drop-off position," and the processed sample container 4 is removed by an external mechanism or manually. It can be considered that, compared to the implementation methods in related technologies that rely on bottom mechanical transmission or split devices, this application achieves wear-free transmission and axial stability control of the sample container through the collaborative design of the rotary drive unit (as a top non-contact magnetic drive mechanism) and the driven rotation of the bottom (low-friction) bearing of the container stage. In this case, the bottom bearing plays a limiting role. The entire technical solution not only eliminates leakage caused by the opening in the vacuum chamber (maintaining stable vacuum), but also compresses the axial space of the equipment by more than 40%, making it suitable for integration into the end effector of the robotic arm in automated production lines.
[0040] To verify that the device of this application has excellent degassing effect, the following embodiments are also provided.
[0041] Example 1
[0042] The sample to be degassed was diluted brine, which was a mixture of brine and deionized water at a volume ratio of 1:50. The diluted brine was used for density detection with an external density meter, and degassing it (including removing carbon dioxide) improved detection accuracy. 125 ml of the diluted brine was placed in a sample container, and the diluted brine was degassed according to the workflow of the integrated degassing and mixing system described above. The vacuum degree of the sealed chamber was set to -70 kPa. The rotary motor was started at 300 rpm, rotating alternately in both directions (e.g., 10 seconds forward → 1 second stop → 10 seconds reverse) for 5 cycles. Simultaneous degassing and mixing were performed at room temperature for 10 minutes. After degassing, the dissolved C in the diluted brine... The concentration decreased.
[0043] The degassed and diluted brine was injected into an external high-precision vibrating tube density meter (Anton Paar DMA 5001M, accuracy ±0.0001 g / cm³). 3 The density at room temperature was measured to be 1.0234 g / cm³. 3 The density of the theoretical aerated brine is 1.0235 g / cm³. 3 The deviation was only 0.005%, while the density of the diluted brine without degassing was 0.12% lower, at 1.0223 g / cm³, due to interference from residual CO2 microbubbles. 3 .
[0044] The above degassing and density value test process was repeated 5 times, and the RSD of the parallel measurements was ≤0.002%, which verified the reliability of the degassing process for density measurement. This method eliminates the significant impact of inaccurate density measurement on subsequent calculation results.
[0045] Example 2
[0046] The sample to be degassed is the ion chromatography eluent. Degassing it helps avoid column gas resistance and improves retention time. The ion chromatography eluent is prepared by dissolving sodium carbonate and sodium hydroxide in 1 L of ultrapure water, with a sodium carbonate concentration of 7.5 mmol / L and a sodium hydroxide concentration of 0.75 mmol / L. The ion chromatography eluent is placed in a sample container, and degassed according to the workflow of the integrated degassing and mixing system described above. The vacuum degree of the sealed chamber is set to -70 kPa. The rotary motor is started at 400 rpm, rotating alternately in both directions (e.g., 20 s forward → 1 s pause → 20 s reverse), for 5 cycles. Simultaneous degassing and mixing are performed at room temperature for 10 minutes. After degassing, the concentration of dissolved gases in the ion chromatography eluent decreases.
[0047] The assay was performed using a Metropole 940 fully automated dual-channel ion chromatography system, a Metrosep A Supp 16-250 / 4.0 anion exchange column, suppressed conductivity detection, a flow rate of 0.7 mL / min, and an injection volume of 20 μL containing NO. 3- (0.1 ppm), SO4 2- (0.2 ppm) environmental water sample. Compared with the undegassed ion chromatography eluent, the column inlet pressure fluctuation decreased from ±0.3 MPa to ±0.05 MPa, and no baseline jump caused by gas resistance was observed; gradient elution test showed that NO 3- Retention time RSD was optimized from 0.82% to 0.28%, SO4 2- The retention time RSD decreased from 0.75% to 0.31%, verifying that degassing and mixing of the ion chromatography eluent significantly improved the stability of the ion chromatography system.
[0048] Although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
[0049] The detailed descriptions listed above are merely specific descriptions of feasible implementation methods of this application and are not intended to limit the scope of protection of this application. All equivalent implementation methods or modifications made without departing from the spirit of the art of this application should be included within the scope of protection of this application.
Claims
1. An integrated degassing and mixing device, characterized in that, include: A container stage, at least for supporting a sample container, is disposed on a first working surface, the sample container being used to hold a sample to be degassed; A sealing unit, at least for sealing the opening of the sample container, so that the inner cavity of the sample container is formed as a closed cavity; A lifting drive unit is connected to the sealing unit and is at least used to drive the sealing unit to move along the second working surface between the first working position and the second working position. At the first working position, the sealing unit seals the opening of the sample container, and at the second working position, the sealing unit moves away from the opening of the sample container. The second working surface is perpendicular to the first working surface. A rotary drive unit, connected to the sample container, is used at least to drive the sample container sealed by the sealing unit to rotate; A vacuum unit, connected to the enclosed cavity, is used at least to establish and maintain a negative pressure environment within the enclosed cavity.
2. The integrated degassing and mixing device according to claim 1, characterized in that, It also includes a horizontal drive unit, which includes a guide rail and a drive mechanism. The guide rail extends along the first working surface, and the container platform is movably disposed on the guide rail. The drive mechanism is used to drive the container platform to approach or move away from the first work station along the guide rail.
3. The integrated degassing and mixing device according to claim 2, characterized in that, The drive mechanism is a servo motor or a stepper motor.
4. The integrated degassing and mixing device according to claim 1, characterized in that, The sealing unit is provided with a through hole, and the vacuum unit is connected to the closed cavity through the through hole.
5. The integrated degassing and mixing device according to claim 4, characterized in that, The device also includes a high-speed rotary joint disposed on the through hole, and the vacuum unit is connected to the sealing unit through the high-speed rotary joint.
6. The integrated degassing and mixing device according to claim 1, characterized in that, The device also includes a clamping unit located on the second working surface and below the sealing unit for clamping or releasing the sample container.
7. The integrated degassing and mixing device according to claim 6, characterized in that, The clamping unit is equipped with a pressure sensor to provide real-time feedback on the clamping status of the clamping unit.
8. The integrated degassing and mixing device according to claim 1, characterized in that, The container stage is equipped with a rotatable cylindrical structure including a bottom bearing. The cylinder of the rotatable cylindrical structure has a built-in slot design for adapting to the sample container, and the bottom bearing is used to provide support for the sample container.
9. An integrated degassing and mixing system, characterized in that, The device includes the integrated degassing and mixing apparatus according to any one of claims 1-8, a first workbench and a second workbench; wherein the container platform and the lifting drive unit are respectively disposed on the first workbench and the second workbench.
10. A method of using an integrated degassing and mixing system, characterized in that, Includes the following steps: S1. Place the sample container of the sample to be degassed on the container platform of the first workbench; S2. The horizontally driven container stage moves along the first worktable to the preset working position directly below the sealing unit; S3. The sealing unit and the rotary drive unit located on the second worktable are driven to descend vertically, so that the sealing unit and the sample container are sealed to form a closed cavity. S4. Start the vacuum unit to create and maintain a negative pressure environment by drawing a vacuum in the sealed cavity through the sealing unit. The rotary drive unit is activated to drive the sealing unit and sample container to rotate, so that the sample to be degassed in the sample container forms a vortex and achieves uniform mixing. The rotary drive unit periodically switches directions according to a preset program. S5. Shut down the vacuum unit to break the negative pressure environment inside the sealed cavity; S6. The sealing unit and the rotary drive unit are driven to rise vertically by the lifting drive unit, so that the sealing unit is separated from the sample container. S7. The horizontally driven container stage moves along the first worktable to the initial position to remove the processed sample container.