Nuclear magnetic resonance tube cleaning device and cleaning method

Abstract

This invention discloses an NMR tube cleaning device and method, belonging to the field of NMR tube cleaning technology. The NMR tube cleaning device includes a tube rack, an air blowing assembly, a first liquid return assembly, and a liquid filling assembly. The NMR tube is placed on the tube rack, and a liquid guide tube extends into the NMR tube. The air blowing assembly is used to fill the NMR tube with gas, so that the residual liquid inside the NMR tube flows through the liquid guide tube to the first liquid return assembly, and the type of residual liquid is matched with the type of the first liquid return assembly. The liquid filling assembly is used to fill the liquid guide tube with cleaning fluid, so that the cleaning fluid soaks the inner wall of the NMR tube. The air blowing assembly is also used to fill the NMR tube with gas, so that the cleaning fluid flows through the liquid guide tube to the outside of the NMR tube and is collected separately, and the type of cleaning fluid is matched with the type of residual liquid. Beneficial effects: Less cleaning fluid is used, it does not damage the NMR tube, and it can separately collect residual liquid and cleaning fluid, avoiding resource waste.

Description

Technical Field

[0001] This invention relates to the field of nuclear magnetic resonance tube cleaning technology, and in particular to a nuclear magnetic resonance tube cleaning device and cleaning method. Background Technology

[0002] In chemical research, nuclear magnetic resonance (NMR) technology is a widely used testing technique that provides crucial information for the structural analysis of compounds. During the testing process, the sample is placed in an NMR tube and the NMR tube is placed in a magnet for detection. Cleaning the NMR tube is a very important part; incomplete cleaning or improper cleaning methods can affect the experimental results.

[0003] Currently, cleaning brushes, liquid guide tubes, and three-dimensional positioning devices are commonly used to clean NMR tubes. However, this method can easily damage the inner wall of the NMR tube with the cleaning brushes, and the amount of solvent used in the cleaning solution is relatively large. Moreover, the above cleaning methods do not consider the recovery of the cleaning solution and the relatively expensive residual liquid inside the NMR tube, resulting in a waste of resources.

[0004] In summary, there is an urgent need to design a nuclear magnetic resonance tube cleaning device and cleaning method to solve the above problems. Summary of the Invention

[0005] The purpose of this invention is to provide a nuclear magnetic resonance tube cleaning device and cleaning method that uses less cleaning fluid, does not damage the nuclear magnetic resonance tube, and can separately classify and recycle residual liquid and cleaning fluid to avoid resource waste.

[0006] To achieve this objective, the present invention adopts the following technical solution:

[0007] Nuclear magnetic resonance tube cleaning device, including:

[0008] A tube rack, on which nuclear magnetic resonance tubes are placed, and a liquid guide tube extends into the nuclear magnetic resonance tube;

[0009] The gas blowing assembly and the first liquid return assembly are provided. The gas blowing assembly is used to fill the NMR tube with gas so that the residual liquid in the NMR tube flows through the liquid guide tube to the first liquid return assembly. The type of the residual liquid is matched with the first liquid return assembly.

[0010] The liquid filling assembly is used to fill the liquid guide tube with cleaning fluid so that the cleaning fluid soaks the inner wall of the NMR tube, and the air blowing assembly is also used to fill the NMR tube with gas so that the cleaning fluid flows through the liquid guide tube to the outside of the NMR tube and is collected separately, and the type of the cleaning fluid is matched with the type of the residual liquid.

[0011] Furthermore, the NMR tube cleaning device also includes a robotic arm, which is used to remove the cap of the NMR tube to be cleaned, so that the robotic arm can extend the liquid guide tube into the NMR tube, and the color of the cap is set to match the type of the residual liquid;

[0012] The robotic arm includes:

[0013] The robotic arm body is disposed on one side of the tube rack, and a negative pressure port is provided at the free end of the robotic arm body for adsorbing the tube cap;

[0014] The cap removal claw is retractable and mounted on the main body of the robotic arm and located on the outer periphery of the negative pressure port. The cap removal claw is used to remove the cap from the nuclear magnetic tube when the cap is attracted to the negative pressure port.

[0015] The free end of the robotic arm body is provided with a sealing plug and a liquid guide tube. The sealing plug is used to seal the opening of the nuclear magnetic resonance tube, and the liquid guide tube passes through the sealing plug and can move relative to the sealing plug within the nuclear magnetic resonance tube.

[0016] Furthermore, the air blowing assembly includes:

[0017] A first gas source and a first valve, one end of the first valve is connected to the first gas source, and the other end of the first valve is connected to the nuclear magnetic resonance tube, so that the gas from the first gas source is blown into the nuclear magnetic resonance tube. The first valve is used to control the connection and disconnection between the first gas source and the nuclear magnetic resonance tube.

[0018] Furthermore, the nuclear magnetic resonance tube cleaning device also includes a transfer valve, one end of which is connected to the liquid guide tube; the first return liquid assembly includes:

[0019] The second valve, the other end of which is selectively connected to one end of the second valve;

[0020] Multiple first recovery units are provided, and the other end of the second valve is connected to each of the first recovery units respectively. The second valve is capable of selectively connecting one of the first recovery units according to the type of the residual liquid, so that one type of the residual liquid is recovered in one of the first recovery units.

[0021] A first exhaust component, wherein one first recovery component is connected to a first exhaust component, and activated carbon is disposed in the exhaust port of the first exhaust component; and / or

[0022] A condenser is provided between the first recovery unit and the first exhaust unit for condensing the gas.

[0023] Furthermore, the NMR tube cleaning apparatus further includes a first distillation assembly for classifying and distilling the residual liquid within each of the first recovery units and collecting it; the first distillation assembly includes:

[0024] A first distillation valve and a first distiller, wherein one end of the first distillation valve is selectively connected to each of the first recovery components, and the other end of the first distillation valve is connected to one end of the first distiller;

[0025] Multiple collection devices are provided, with the other end of the first distiller selectively connected to each of the collection devices, so that a distilled residue is collected in one of the collection devices.

[0026] Furthermore, the liquid filling assembly includes:

[0027] A drive unit and a third valve, wherein the two ends of the drive unit are respectively connected to the transfer valve and the third valve, and the transfer valve can selectively connect to the drive unit;

[0028] Multiple filling elements are provided, and the third valve is connected to each of the filling elements respectively. The third valve can selectively connect to one of the filling elements according to the type of residual liquid, so that the driving element drives the cleaning liquid in one of the filling elements to the liquid guide tube.

[0029] Furthermore, the NMR tube cleaning device also includes a second liquid return assembly. When the air blowing assembly fills the NMR tube with gas, the cleaning solution after immersing the NMR tube can flow through the liquid guide tube into the second liquid return assembly. The second liquid return assembly includes:

[0030] The fourth valve, the other end of which can be selectively connected to one end of the fourth valve;

[0031] Multiple second recovery units are provided, and the other end of the fourth valve is connected to each of the second recovery units respectively. The fourth valve can selectively connect to one of the second recovery units according to the type of the cleaning fluid, so that one type of cleaning fluid is recovered in one of the second recovery units, and one second recovery unit is correspondingly provided with one filling unit.

[0032] In one of the second recovery components, a first exhaust component is provided, and the condenser is selectively provided between the second recovery component and the first exhaust component.

[0033] Furthermore, the NMR tube cleaning apparatus further includes a second distillation assembly for separately distilling the cleaning solution within each of the second recovery units; the second distillation assembly includes:

[0034] A second distillation valve and a second distiller, wherein one end of the second distillation valve is selectively connected to each of the second recovery components, the other end of the second distillation valve is connected to one end of the second distiller, and the other end of the second distiller is selectively connected to each of the liquid filling components.

[0035] Furthermore, the NMR tube cleaning device also includes a drying assembly for drying residual liquid inside the NMR tube and the liquid guide tube after cleaning; the drying assembly includes:

[0036] A heating element and a second gas source are provided. The two ends of the heating element are respectively connected to the second gas source and the transfer valve. The transfer valve is selectively connected to the heating element. The heating element is used to heat the gas supplied by the second gas source and to allow the heated gas to flow into the liquid guide tube to dry the residual liquid in the nuclear magnetic resonance tube and the liquid guide tube. When the residual liquid is dried, the liquid guide tube selectively moves upward back to its initial position.

[0037] A fifth valve and a second exhaust device, the two ends of the fifth valve being connected to the inside of the nuclear magnetic resonance tube and the second exhaust device respectively, to discharge the heating gas used to dry the residual liquid inside the nuclear magnetic resonance tube and the liquid guide tube.

[0038] A method for cleaning nuclear magnetic resonance (NMR) tubes, based on the NMR tube cleaning apparatus described above, includes the following steps:

[0039] S1: The blowing assembly fills the NMR tube with gas so that the residual liquid in the NMR tube is sorted and flowed into the first return liquid assembly through the liquid guide tube;

[0040] S2: Then, the liquid filling assembly fills the liquid guide tube with the cleaning solution so that the cleaning solution soaks the inner wall of the nuclear magnetic tube.

[0041] S3: After soaking is completed, the air blowing assembly is used to fill the NMR tube with gas so that the cleaning solution flows out of the NMR tube through the liquid guide tube, and the cleaning solution is sorted and recycled.

[0042] The beneficial effects of this invention are as follows:

[0043] By using an air-blowing assembly to inject gas into the NMR tube, the residual liquid inside the NMR tube is separated and flows through a liquid guide tube to the first liquid return assembly, thus achieving the classified recovery of the relatively expensive residual liquid inside the NMR tube. Next, a liquid filling assembly fills the liquid guide tube with cleaning fluid, allowing the cleaning fluid to soak and clean the inner wall of the NMR tube. Finally, the air-blowing assembly injects gas into the NMR tube again, allowing the cleaning fluid, after soaking the NMR tube, to flow through a liquid guide tube to the outside of the NMR tube, thereby achieving automatic cleaning of the NMR tube. This method achieves two advantages: firstly, it allows for the separate recovery of residual liquid and cleaning fluid, resulting in high recovery value; secondly, it enables the cleaning of the NMR tube through a cleaning method that soaks the corresponding residual liquid with cleaning fluid, resulting in good cleaning effect and low cleaning fluid consumption. It also eliminates the need for a cleaning brush, thus avoiding damage to the NMR tube.

[0044] The nuclear magnetic resonance tube cleaning method of the present invention, based on the above-mentioned nuclear magnetic resonance tube cleaning device, is simple and convenient to operate, has a good cleaning effect, uses less cleaning fluid, will not damage the nuclear magnetic resonance tube, and can separately classify and recycle residual liquid and cleaning fluid, avoiding resource waste, and can avoid environmental pollution caused by directly discharging residual liquid and cleaning fluid without recycling. Attached Figure Description

[0045] Figure 1 This is a schematic diagram of the structure of the nuclear magnetic resonance tube cleaning device provided by the present invention;

[0046] Figure 2 This is a schematic flowchart of the nuclear magnetic resonance tube cleaning method provided by the present invention.

[0047] In the picture:

[0048] 1-Tube rack; 2-NMR tube; 3-Liquid delivery tube; 4-Robot arm;

[0049] 5-Blowing assembly; 51-First air source; 52-First valve;

[0050] 6-First return liquid assembly; 61-Second valve; 62-First recovery component; 63-First venting component;

[0051] 7-Filling assembly; 71-Driver; 72-Third valve; 73-Filling component;

[0052] 8-Transfer valve;

[0053] 91-First distillation valve; 92-First distiller; 93-First collection valve; 94-Collection piece;

[0054] 10-Second return liquid assembly; 11-Fourth valve; 12-Second recovery component;

[0055] 21-Second distillation valve; 22-Second distiller; 23-Second collection valve;

[0056] 31-Heating element; 32-Second air source; 33-Fifth valve; 34-Second exhaust element. Detailed Implementation

[0057] All features disclosed in this specification, or all steps in all disclosed methods or processes, may be combined in any way, except for mutually exclusive features and / or steps.

[0058] Any feature disclosed in this specification, unless specifically stated otherwise, may be replaced by other equivalent or similar features. That is, unless specifically stated otherwise, each feature is merely one example of a series of equivalent or similar features. Throughout this specification, the same reference numerals indicate the same elements.

[0059] To make the technical problems solved by the present invention, the technical solutions adopted, and the technical effects achieved clearer, the technical solutions of the present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.

[0060] Example 1

[0061] This embodiment proposes an NMR tube cleaning device. This device is used to clean NMR tubes and can separately recover the cleaning solution and the relatively expensive residual liquid inside the NMR tube, avoiding resource waste. Specifically, the residual liquid inside the NMR tube refers to a deuterated solvent, such as deuterated chloroform solution, heavy water solution, deuterated DMSO solution, or other common deuterated solvents. The cleaning solution can be a non-deuterated solvent compatible with the deuterated solvent, such as chloroform solution, water, DMSO solution, or other common solvents. For example, when the residual liquid inside the NMR tube is a deuterated chloroform solution, the NMR tube needs to be soaked and dissolved using a chloroform cleaning solution.

[0062] Specifically, such as Figure 1As shown, the NMR tube cleaning device includes a tube rack 1, an air blowing assembly 5, a first liquid return assembly 6, and a liquid filling assembly 7. Multiple NMR tubes 2 to be cleaned and / or multiple cleaned NMR tubes 2 are placed on the tube rack 1, and a liquid guide tube 3 extends into each NMR tube 2. The air blowing assembly 5 is used to fill the NMR tube 2 with gas, so that the residual liquid in the NMR tube 2 can flow through the liquid guide tube 3 to the first liquid return assembly 6 under the action of the gas. The type of residual liquid is matched with the first liquid return assembly 6 to achieve classified recovery of the residual liquid. The liquid filling assembly 7 is used to fill the liquid guide tube 3 with cleaning fluid, so that the cleaning fluid soaks the inner wall of the NMR tube 2. After a preset soaking time, the air blowing assembly 5 is also used to fill the NMR tube 2 with gas, so that the cleaning fluid can flow through the liquid guide tube 3 to the outside of the NMR tube 2 under the action of the gas and be collected classified. The type of cleaning fluid is matched with the type of residual liquid, that is, one type of residual liquid requires a corresponding type of cleaning fluid for cleaning, thereby ensuring a good cleaning effect on the NMR tube 2.

[0063] By introducing gas into the NMR tube 2 through the air blowing assembly 5, the residual liquid inside the NMR tube 2 is separated and flows through the liquid guide tube 3 to the first liquid return assembly 6, thereby achieving the classified recovery of the relatively expensive residual liquid inside the NMR tube 2. Then, the liquid filling assembly 7 introduces cleaning fluid into the liquid guide tube 3, so that the cleaning fluid soaks and cleans the inner wall of the NMR tube 2. Finally, the air blowing assembly 5 introduces gas into the NMR tube 2 again, so that the cleaning fluid after soaking the NMR tube 2 flows out of the NMR tube 2 through the liquid guide tube 3, thereby achieving automatic cleaning of the NMR tube 2. Using the above method, on the one hand, the residual liquid and cleaning fluid can be classified and recovered separately, which has a high recovery value. On the other hand, the NMR tube 2 can be cleaned by soaking the corresponding residual liquid with a cleaning fluid, which has a good cleaning effect and uses less cleaning fluid. It does not require the use of a cleaning brush, so as to avoid damage to the NMR tube 2.

[0064] Furthermore, throughout the cleaning process, there is no need to remove or place the NMR tubes 2. The NMR tubes 2 can be cleaned simply by keeping them resting on the tube rack 1. This makes the cleaning operation simple and convenient, and avoids damage to the NMR tubes 2 during movement, thus better protecting them. In addition, the tube rack 1 can be used as a support during cleaning, as well as for routine sample preparation or temporary collection and storage of the NMR tubes 2, facilitating easy access and diversifying its functionality. In this embodiment, a tube rack 1 with dimensions of (10 tubes * φ0.5) * (10 tubes * φ0.5) can be used.

[0065] It is worth noting that the types of residual solutions and cleaning solutions are set in a related manner. That is, the residual solutions mostly use deuterated solvents such as deuterated chloroform, heavy water, or deuterated DMSO. Correspondingly, the same non-deuterated solvents such as non-deuterated chloroform, water, or non-deuterated DMSO are used to clean the NMR tube 2. This allows the same non-deuterated solvent to dissolve the trace amounts of solute remaining on the inner wall of the NMR tube 2, while reducing the amount of cleaning solution used and cleaning the NMR tube 2 more quickly.

[0066] Furthermore, the same non-deuterium solvent can be used to dissolve and clean the NMR tube 2 multiple times without causing solute to precipitate in the residual liquid due to the difference in solubility between the cleaning solution and the residual liquid. Therefore, there is no need for friction cleaning with a cleaning brush, and the amount of non-deuterium solvent used to clean one NMR tube 2 is small, about the volume of three to five NMR tubes 2 (approximately 6 mL to 7 mL). Moreover, the non-deuterium solvent containing a small amount of solute will be automatically sorted and collected, and will not remain in the NMR tube 2, so as to ensure the cleaning effect of the NMR tube 2.

[0067] It is worth noting that using a non-deuterium solvent to dissolve and clean the NMR tube 2 multiple times specifically refers to gradually filling the NMR tube 2 with cleaning solution and immersing it in the solution multiple times. For example, the first time, half the volume of cleaning solution is filled into the NMR tube 2; the second time, three-quarters of the volume is filled; and the third time, the NMR tube 2 is filled completely. This method of immersing in small amounts multiple times ensures a good dissolution effect on the NMR tube 2 without wasting cleaning solution, thus guaranteeing a good cleaning effect. In this embodiment, the NMR tube 2 is filled with cleaning solution twice to ensure a better cleaning effect.

[0068] Specifically, such as Figure 1 As shown, the NMR tube cleaning device also includes a robotic arm 4, which is located on one side of the tube rack 1, with a liquid guide tube 3 mounted on it. The robotic arm 4 is used to remove the cap of the NMR tube 2 to be cleaned, allowing it to extend the liquid guide tube 3 into the NMR tube 2. The color of the cap matches the type of residual liquid, meaning one color cap corresponds to one type of residual liquid. During the cleaning process, the specific type of residual liquid can be identified by detecting the color of the cap. A drive motor can be installed on the robotic arm 4 to move the liquid guide tube 3 into the NMR tube 2. The liquid guide tube 3 is typically located at the bottom of the NMR tube 2 to ensure effective liquid guidance.

[0069] Specifically, the robotic arm 4 includes a robotic arm body and a cap-removing claw; the robotic arm body is located on one side of the tube rack 1, and a negative pressure port is provided at the free end of the robotic arm body for vacuum adsorption of tube caps; the cap-removing claw is retractably mounted on the robotic arm body and located on the outer periphery of the negative pressure port. The robotic arm body can be a six-axis robotic arm commonly used in existing technologies.

[0070] When the free end of the robotic arm moves above the NMR tube 2, the robotic arm can identify the color of the tube cap (the color of the tube cap is related to the residual liquid used in the NMR tube 2); then it opens the negative pressure port to vacuum-adhere the tube cap; at the same time, it releases the cap removal claw so that the cap removal claw can detach the tube cap from the NMR tube 2, thereby removing the tube cap from the NMR tube 2; then it moves the tube cap into the NMR cap storage tank to achieve unified collection of the tube caps; finally, it closes the negative pressure port and retracts the cap removal claw.

[0071] Furthermore, such as Figure 1 As shown, a sealing plug and the aforementioned liquid guide tube 3 are also provided at the free end of the robotic arm body. The sealing plug is used to seal the opening of the NMR tube 2 to prevent the liquid inside the NMR tube 2 from overflowing to the outside of the NMR tube 2, thereby preventing the overflowing liquid from contaminating the outer wall of the NMR tube 2 and the tube frame 1. The liquid guide tube 3 passes through the sealing plug and can move relative to the sealing plug within the NMR tube 2, allowing it to move to the bottom of the NMR tube 2 under the drive of a drive motor. In this embodiment, the sealing plug can specifically be a rubber plug.

[0072] Specifically, such as Figure 1 As shown, the air blowing assembly 5 includes a first air source 51 and a first valve 52. One end of the first valve 52 is connected to the first air source 51, and the other end of the first valve 52 is sealed to the inside of the NMR tube 2, so that the gas provided by the first air source 51 can be blown into the NMR tube 2 through the first valve 52. The first valve 52 is used to control the connection between the first air source 51 and the NMR tube 2. Specifically, the first air source 51 can be a dry air compressor or an inert air source, that is, the gas provided by the first air source 51 has a certain pressure to facilitate the movement of the liquid in the NMR tube 2 along the liquid guide tube 3. The first valve 52 can be a commonly used on / off valve in the prior art. In addition, the main body of the robot is also provided with an air blowing port that connects to the sealing plug and is connected to the inside of the NMR tube 2. The other end of the first valve 52 is connected to the air blowing port to achieve a sealed connection between the other end of the first valve 52 and the inside of the NMR tube 2.

[0073] Furthermore, such as Figure 1As shown, the nuclear magnetic resonance tube cleaning device also includes a transfer valve 8, one end of which is sealed and connected to the liquid guide tube 3. Furthermore, the first return liquid assembly 6 includes a second valve 61 and multiple first recovery components 62. The other end of the transfer valve 8 can selectively connect to one end of the second valve 61. Multiple first recovery components 62 are arranged side-by-side and independently. The other end of the second valve 61 is connected to each of the first recovery components 62. The second valve 61 can selectively connect to a corresponding first recovery component 62 based on the type of residual liquid or the color of the tube cap, so that one type of residual liquid is recovered within each first recovery component 62, thereby achieving the classified recovery of various residual liquids. In this embodiment, the first recovery component 62 can specifically be a storage tank, and four first recovery components 62 are provided.

[0074] Specifically, such as Figure 1 As shown, the first liquid return assembly 6 also includes a first exhaust component 63. A first exhaust component 63 is connected to a first recovery component 62 to discharge gas entering the first recovery component 62, preventing excessive gas pressure within the first recovery component 62. Furthermore, activated carbon is provided in the exhaust port of the first exhaust component 63 to adsorb harmful impurities in the gas, ensuring that the gas discharged through the exhaust port is environmentally friendly. In this embodiment, the first exhaust component 63 can specifically be an exhaust pipe.

[0075] Furthermore, the first liquid return assembly 6 also includes a condenser, which is selectively provided between the first recovery unit 62 and the first exhaust unit 63 for condensing the gas. Since a small portion of the low-boiling-point residual liquid, such as deuterated chloroform, deuterated acetone, and deuterated dichloromethane, will vaporize into gas during the flow process, when the gas in the first recovery unit 62 passes through the condenser, the condenser can condense the low-boiling-point solution from the gas, so that the condensed solution can flow back into the first recovery unit 62, avoiding the direct discharge of the low-boiling-point residual liquid and thus preventing environmental pollution. It can also recover the residual liquid in the largest possible amount, thereby achieving the purpose of environmental protection and emission reduction of residual liquid.

[0076] In order to enable the recovered residual liquid to be reused, the NMR tube cleaning device in this embodiment also includes a first distillation assembly for classifying and distilling the residual liquid in each first recovery unit 62 and collecting it separately, so as to facilitate the reuse of the residual liquid.

[0077] Specifically, such as Figure 1As shown, the first distillation assembly includes a first distillation valve 91, a first distiller 92, and multiple collection units 94 arranged in parallel. One end of the first distillation valve 91 is selectively connected to each of the first recovery units 62, and the other end of the first distillation valve 91 is connected to one end of the first distiller 92. The other end of the first distiller 92 is selectively connected to each of the collection units 94, meaning that one first recovery unit 62 is correspondingly paired with one collection unit 94, so that one collection unit 94 collects a single distillation residue. A first collection valve 93 is provided between the first distiller 92 and the multiple collection units 94, allowing the first distiller 92 to be selectively connected to one collection unit 94. In this embodiment, the first distiller 92 can specifically be a flash evaporator, an evaporator, or a distillation unit; the collection unit 94 can specifically be a storage tank, and four collection units 94 are provided.

[0078] It is worth noting that a liquid level sensor is installed in each first recovery unit 62. The liquid level sensor is used to detect the liquid level in the first recovery unit 62. When the liquid level in one of the first recovery units 62 reaches a preset height, the first recovery unit 62 is connected to the first distiller 92 through the first distillation valve 91, so that the residual liquid in the first recovery unit 62 can be automatically discharged into the first distiller 92 for distillation and recovery.

[0079] Specifically, such as Figure 1 As shown, the liquid filling assembly 7 includes a drive unit 71, a third valve 72, and multiple liquid filling components 73. The two ends of the drive unit 71 are connected to a transfer valve 8 and the third valve 72, respectively. The transfer valve 8 can selectively connect to the drive unit 71. Multiple liquid filling components 73 are arranged in parallel and independently. The third valve 72 is connected to each liquid filling component 73. Each liquid filling component 73 corresponds to a type of residual liquid or the color of a tube cap. The third valve 72 can selectively connect to a liquid filling component 73 according to the type of residual liquid or the color of the tube cap, so that the drive unit 71 drives the cleaning liquid in one liquid filling component 73 into the liquid guide tube 3, thereby immersing and dissolving the inner wall of the NMR tube 2 with the cleaning liquid, thus achieving the cleaning of the NMR tube 2. In this embodiment, the drive unit 71 can specifically be a liquid peristaltic pump or a plunger pump, and the liquid filling component 73 can specifically be a liquid storage tank. Four liquid filling components 73 are specifically provided.

[0080] Furthermore, such as Figure 1 As shown, the NMR tube cleaning device also includes a second liquid return assembly 10. After the soaking and cleaning is completed, the air blowing assembly 5 fills the NMR tube 2 with gas so that the cleaning liquid after soaking the NMR tube 2 can flow through the liquid guide tube 3 to the second liquid return assembly 10 in a classified manner, so as to realize the classified collection of the cleaning liquid.

[0081] Specifically, such as Figure 1As shown, the second return fluid assembly 10 includes a fourth valve 11 and multiple parallel and independently arranged second recovery components 12. The other end of the transfer valve 8 can selectively connect to one end of the fourth valve 11, and the other end of the fourth valve 11 is connected to each of the second recovery components 12. The fourth valve 11 can selectively connect to one second recovery component 12 according to the specific type of cleaning fluid, so that one type of cleaning fluid is recovered within each second recovery component 12, thereby achieving classified collection of the cleaning fluid. Each second recovery component 12 is correspondingly arranged with one filling component 73. In this embodiment, the second recovery component 12 can specifically be a storage tank.

[0082] Furthermore, such as Figure 1 As shown, a first exhaust vent 63 is provided on a second recovery unit 12 to exhaust the gas entering the second recovery unit 12 and prevent excessive gas pressure inside the second recovery unit 12; and, a condenser is selectively provided between the second recovery unit 12 and the first exhaust vent 63 so that the condenser can condense the solution with a lower boiling point from the gas, thereby allowing the condensed solution to flow back into the second recovery unit 12, preventing the cleaning liquid with a lower boiling point from being directly discharged and polluting the environment, and enabling the maximum recovery of the cleaning liquid, thereby achieving the purpose of environmental protection and emission reduction of the cleaning liquid.

[0083] In order to enable the recovered cleaning fluid to be recycled, the NMR tube cleaning device in this embodiment also includes a second distillation component for classifying and distilling the cleaning fluid in each of the second recovery units 12, so that the distilled cleaning fluid can enter the corresponding filling unit 73 for recycling.

[0084] Specifically, such as Figure 1 As shown, the second distillation assembly includes a second distillation valve 21 and a second distiller 22. One end of the second distillation valve 21 is selectively connected to each of the second recovery units 12, and the other end of the second distillation valve 21 is connected to one end of the second distiller 22. The other end of the second distiller 22 is selectively connected to each of the filling units 73, so that the cleaning solution in one of the second recovery units 12 enters the corresponding filling unit 73 after passing through the second distiller 22, thereby realizing the recycling of the cleaning solution. A second collection valve 23 is provided between the second distiller 22 and the multiple filling units 73, so that the second distiller 22 can be selectively connected to one filling unit 73 through the second collection valve 23. In this embodiment, the second distiller 22 can specifically be a flash evaporator, an evaporator, or a distillation unit.

[0085] It is worth noting that each of the second recovery units 12 is equipped with the aforementioned liquid level sensor to detect the liquid level within the second recovery unit 12. When the liquid level in one of the second recovery units 12 reaches a preset height, that second recovery unit 12 is connected to the second distiller 22 via the second distillation valve 21, thereby automatically discharging the cleaning solution within the second recovery unit 12 into the second distiller 22 for distillation and recovery. In this embodiment, four second recovery units 12 are provided.

[0086] Furthermore, the NMR tube cleaning device also includes a drying component, which is used to dry the residual liquid inside the NMR tube 2 and the liquid guide tube 3 after cleaning, so that the NMR tube 2 and the liquid guide tube 3 remain dry. This allows the NMR tube 2 to be directly used for the next time without the need for additional drying. The residual liquid mainly refers to the cleaning fluid and contains a very small amount of residual liquid.

[0087] Specifically, such as Figure 1 As shown, the drying assembly includes a heating element 31, a second gas source 32, a fifth valve 33, and a second exhaust valve 34. The heating element 31 is connected at both ends to the second gas source 32 and a transfer valve 8, respectively. The transfer valve 8 is selectively connected to the heating element 31. The heating element 31 heats the gas supplied by the second gas source 32 and allows the heated gas to flow into the liquid guide tube 3, thereby drying the residual liquid inside the NMR tube 2 and the liquid guide tube 3, thus keeping the NMR tube 2 and the liquid guide tube 3 dry. The fifth valve 33 is connected at both ends to the interior of the NMR tube 2 and the second exhaust valve 34, respectively, to discharge the heating gas used to dry the residual liquid inside the NMR tube 2 and the liquid guide tube 3 through the second exhaust valve 34, ensuring that the gas pressure inside the NMR tube 2 is suitable.

[0088] In this embodiment, activated carbon for adsorbing harmful impurities is provided in the exhaust port of the second exhaust component 34. The heating component 31 can be an electric heater, and the second air source 32 can be a drying air compressor or an inert air source. That is, the gas provided by the second air source 32 has a certain pressure to dry the residual liquid in the NMR tube 2 and the liquid guide tube 3. The fifth valve 33 can be a commonly used on / off valve in the prior art. The main body of the robot is also provided with an exhaust port that connects to the sealing plug and is connected to the inside of the NMR tube 2. The fifth valve 33 is connected to the exhaust port to achieve a sealed connection between the fifth valve 33 and the inside of the NMR tube 2.

[0089] Furthermore, since the residual liquid with a high boiling point tends to move upwards along the walls of the NMR tube 2 and the liquid guide tube 3 when drying the residual liquid, the drive motor can smoothly and selectively move the liquid guide tube 3 back to its initial position during the drying process. This allows the open area at the bottom of the NMR tube 2 to gradually increase, enabling more heating gas to accumulate at the bottom of the NMR tube 2, thus improving the drying effect on the upward-moving residual liquid. In addition, as the liquid guide tube 3 gradually moves upwards, the residual liquid on the liquid guide tube 3 has already been dried, preventing it from splashing onto the tube rack 1 during the movement of the liquid guide tube 3. At the same time, it can speed up the time for the liquid guide tube 3 to move back to its initial position, avoiding the need to move the liquid guide tube 3 back to its initial position after drying is completed.

[0090] Specifically, since the residual liquid is mainly cleaning fluid, the type of cleaning fluid in the NMR tube 2 will affect the drying effect on the NMR tube 2 and the liquid guide tube 3. It is necessary to adjust the heating power of the heating element 31 and the gas supply power of the second gas source 32 according to the boiling point of the specific type of cleaning fluid in the NMR tube 2 in the previous step, so as to ensure the temperature of the gas after being heated by the heating element 31, and thus enable the heating gas at a suitable temperature to dry the residual liquid in the NMR tube 2, ensuring the drying effect.

[0091] Specifically, such as Figure 1 As shown, the aforementioned transfer valve 8, second valve 61, third valve 72, fourth valve 11, first distillation valve 91, second distillation valve 21, first collection valve 93, and second collection valve 23 are all multi-directional valves; and the gas involved can be air or nitrogen.

[0092] Example 2

[0093] This embodiment proposes a method for cleaning nuclear magnetic resonance (NMR) tubes, based on the NMR tube cleaning device described in Embodiment 1, such as... Figure 2 As shown, the process includes the following steps: S1: The blowing assembly 5 fills the NMR tube 2 with gas, so that the residual liquid in the NMR tube 2 flows through the liquid guide tube 3 to the first liquid return assembly 6 in a classified manner, so as to achieve classified collection of the residual liquid; S2: The filling assembly 7 fills the liquid guide tube 3 with cleaning liquid, so that the cleaning liquid soaks the inner wall of the NMR tube 2 to soak and clean the NMR tube 2; S3: After the soaking and cleaning is completed, the blowing assembly 5 fills the NMR tube 2 with gas again, so that the cleaning liquid flows through the liquid guide tube 3 to the outside of the NMR tube 2, and the cleaning liquid is classified and recycled.

[0094] The specific cleaning process of the NMR tube cleaning method in this embodiment is as follows:

[0095] First, close the first valve 52, the transfer valve 8, and the fifth valve 33. When the free end of the robotic arm moves above the NMR tube 2, the robotic arm can identify and record the color of the tube cap. Then, open the negative pressure port on the robotic arm to vacuum-adhere the tube cap. At the same time, release the cap removal claw so that it can detach the tube cap from the NMR tube 2, thereby removing the tube cap from the NMR tube 2. Then, move the tube cap into the NMR cap storage tank to achieve unified collection of the tube caps. Finally, close the negative pressure port and retract the cap removal claw.

[0096] Next, the robotic arm is moved to the opening of the NMR tube 2, and the sealing plug on the robotic arm seals the opening of the NMR tube 2. Then, the liquid guide tube 3 is inserted into the bottom of the NMR tube 2 by the drive motor, and the fifth valve 33 is closed. The transfer valve 8 is connected to the second valve 61, and the second valve 61 is connected to the corresponding first recovery unit 62 according to the color of the tube cap. Then, the first valve 52 is opened so that the first gas source 51 fills the NMR tube 2 with gas through the first valve 52. The residual liquid in the NMR tube 2 flows through the liquid guide tube 3 under the action of the gas to the transfer valve 8, the second valve 61 and the corresponding first recovery unit 62 in sequence. After the gas is circulated for a period of time, the first valve 52 is closed, thus completing the classification and recovery of the residual liquid in the NMR tube 2 into each of the first recovery units 62.

[0097] Then, switch the transfer valve 8 to connect with the drive unit 71, and connect the third valve 72 to the corresponding liquid filling unit 73 according to the color of the tube cap; then, let the drive unit 71 guide the cleaning fluid in the liquid filling unit 73 into the liquid guide tube 3 in sequence through the third valve 72, the drive unit 71 and the transfer valve 8, and then close the drive unit 71 to complete the soaking and cleaning of the nuclear magnetic resonance tube 2.

[0098] Then, after waiting for the cleaning solution to soak the inner wall of the NMR tube 2 for a period of time, the transfer valve 8 is switched to connect with the fourth valve 11, and the fourth valve 11 is connected to the corresponding second recovery unit 12 according to the specific type of cleaning solution. The first valve 52 is then opened so that the first gas source 51 can fill the NMR tube 2 with gas through the first valve 52. This allows the cleaning solution, after soaking the inner wall of the NMR tube 2, to flow through the liquid guide tube 3 to the transfer valve 8, the fourth valve 11 and the corresponding second recovery unit 12 under the action of the gas. After blowing air for a period of time, the first valve 52 is closed to complete the classified recovery of the cleaning solution.

[0099] Then, starting from the step of switching the transfer valve 8 to connect with the drive unit 71, repeat the cycle multiple times, gradually increasing the volume of cleaning fluid introduced into the NMR tube 2 until the NMR tube 2 is filled twice. Ensure that the cleaning fluid is introduced in small amounts and multiple times to soak and clean the NMR tube 2, so as to achieve a better cleaning effect on the NMR tube 2.

[0100] Finally, open the fifth valve 33, switch the transfer valve 8 to connect with the second gas source 32, and adjust the heating power of the heating element 31 and the gas supply power of the second gas source 32 according to the boiling point of the cleaning fluid in the NMR tube 2 used in the previous step, so that the gas heated by the heating element 31 is introduced into the liquid guide tube 3 through the transfer valve 8, thereby allowing the heated gas to dry the residual liquid on the NMR tube 2 and the liquid guide tube 3; at the same time, control the drive motor so that the liquid guide tube 3 can slowly move upward to the initial position, so that the heated gas in the NMR tube 2 can dry the residual liquid moving upward; then close the heating element 31, the second gas source 32 and the fifth valve 33.

[0101] When the liquid level sensor in the first recovery unit 62 or the second recovery unit 12 detects that the liquid level has reached a preset height, the first recovery unit 62 is connected to the first distiller 92 through the first distillation valve 91 (or the second recovery unit 12 is connected to the second distiller 22 through the second distillation valve 21), so that the residual liquid in the first recovery unit 62 and the cleaning liquid in the second recovery unit 12 can be distilled and recovered by the first distiller 92 and the second distiller 22 respectively; then the first distillation valve 91 or the second distillation valve 21 can be closed.

[0102] The above description is only a preferred embodiment of the present invention. For those skilled in the art, there will be changes in the specific implementation and application scope based on the ideas of the present invention. The content of this specification should not be construed as a limitation of the present invention.

Claims

1. A nuclear magnetic resonance tube cleaning device, characterized in that, include: A tube rack (1) on which a nuclear magnetic resonance tube (2) is placed, and a liquid guide tube (3) extends into the nuclear magnetic resonance tube (2); The blowing assembly (5) and the first liquid return assembly (6) are provided. The blowing assembly (5) is used to fill the NMR tube (2) with gas so that the residual liquid in the NMR tube (2) flows through the liquid guide tube (3) to the first liquid return assembly (6). The type of the residual liquid is matched with the first liquid return assembly (6). The liquid filling assembly (7) is used to fill the liquid guide tube (3) with cleaning liquid so that the cleaning liquid soaks the inner wall of the NMR tube (2), and the air blowing assembly (5) is also used to fill the NMR tube (2) with gas so that the cleaning liquid flows through the liquid guide tube (3) to the outside of the NMR tube (2) and is collected separately, and the type of the cleaning liquid is matched with the type of the residual liquid. The nuclear magnetic resonance tube cleaning device also includes a robotic arm (4), which is used to remove the cap of the nuclear magnetic resonance tube (2) to be cleaned so that the robotic arm (4) can extend the liquid guide tube (3) into the nuclear magnetic resonance tube (2), and the color of the cap is set to match the type of the residual liquid; The robotic arm (4) includes: The main body of the robotic arm is disposed on one side of the tube frame (1), and a negative pressure port is provided at the free end of the main body of the robotic arm for adsorbing the tube cap; The cap removal claw can be retracted and set on the main body of the robot and located on the outer periphery of the negative pressure port. The cap removal claw is used to remove the cap from the nuclear magnetic tube (2) when the cap is attracted to the negative pressure port. The free end of the robotic arm body is provided with a sealing plug and a liquid guide tube (3). The sealing plug is used to seal the opening of the nuclear magnetic resonance tube (2). The liquid guide tube (3) passes through the sealing plug and can move relative to the sealing plug within the nuclear magnetic resonance tube (2).

2. The nuclear magnetic resonance tube cleaning apparatus as described in claim 1, characterized in that, The air blowing assembly (5) includes: A first gas source (51) and a first valve (52), one end of the first valve (52) is connected to the first gas source (51), and the other end of the first valve (52) is connected to the nuclear magnetic resonance tube (2) so that the gas from the first gas source (51) is blown into the nuclear magnetic resonance tube (2). The first valve (52) is used to control the connection and disconnection between the first gas source (51) and the nuclear magnetic resonance tube (2).

3. The nuclear magnetic resonance tube cleaning apparatus as described in claim 1 or 2, characterized in that, The nuclear magnetic resonance tube cleaning device further includes a transfer valve (8), one end of which is connected to the liquid guide tube (3); the first return liquid assembly (6) includes: The second valve (61), the other end of the transfer valve (8) is selectively connected to one end of the second valve (61); Multiple first recovery units (62), the other end of the second valve (61) is respectively connected to each of the first recovery units (62), the second valve (61) is capable of selectively connecting one of the first recovery units (62) according to the type of the residual liquid, so that one type of the residual liquid is recovered in one of the first recovery units (62); A first exhaust component (63) is connected to a first recovery component (62), and activated carbon is disposed in the exhaust port of the first exhaust component (63); and / or A condenser is provided between the first recovery unit (62) and the first exhaust unit (63) for condensing the gas.

4. The nuclear magnetic resonance tube cleaning apparatus as described in claim 3, characterized in that, The NMR tube cleaning apparatus further includes a first distillation assembly for classifying and distilling the residual liquid within each of the first recovery units (62) and collecting it; the first distillation assembly includes: A first distillation valve (91) and a first distiller (92), one end of the first distillation valve (91) is selectively connected to each of the first recovery components (62), and the other end of the first distillation valve (91) is connected to one end of the first distiller (92); Multiple collection devices (94), the other end of the first distiller (92) being selectively connected to each of the collection devices (94) so ​​that a distilled residue is collected in one of the collection devices (94).

5. The nuclear magnetic resonance tube cleaning apparatus as described in claim 3, characterized in that, The liquid filling assembly (7) includes: A drive unit (71) and a third valve (72), wherein the two ends of the drive unit (71) are respectively connected to the transfer valve (8) and the third valve (72), and the transfer valve (8) can selectively connect to the drive unit (71); Multiple filling elements (73) are provided, and the third valve (72) is connected to each of the filling elements (73). The third valve (72) can selectively connect to one of the filling elements (73) according to the type of residual liquid, so that the drive (71) drives the cleaning liquid in one of the filling elements (73) into the liquid guide tube (3).

6. The nuclear magnetic resonance tube cleaning apparatus as described in claim 5, characterized in that, The NMR tube cleaning device further includes a second liquid return assembly (10). When the air blowing assembly (5) fills the NMR tube (2) with gas, the cleaning liquid after soaking the NMR tube (2) can flow through the liquid guide tube (3) into the second liquid return assembly (10). The second liquid return assembly (10) includes: The fourth valve (11), the other end of the transfer valve (8) can be selectively connected to one end of the fourth valve (11); Multiple second recovery units (12), the other end of the fourth valve (11) is respectively connected to each of the second recovery units (12), the fourth valve (11) can selectively connect to one of the second recovery units (12) according to the type of the cleaning fluid, so that one type of the cleaning fluid is recovered in one of the second recovery units (12), and one of the second recovery units (12) is correspondingly provided with one of the filling units (73); One of the second recovery components (12) is provided with a first exhaust component (63), and the condenser is selectively provided between the second recovery component (12) and the first exhaust component (63).

7. The nuclear magnetic resonance tube cleaning apparatus as described in claim 6, characterized in that, The nuclear magnetic resonance tube cleaning apparatus further includes a second distillation assembly for distilling the cleaning solution within each of the second recovery units (12); the second distillation assembly includes: The second distillation valve (21) and the second distiller (22) are respectively connected at one end to each of the second recovery components (12), and at the other end of the second distillation valve (21) is connected to one end of the second distiller (22), and at the other end of the second distiller (22) is respectively connected to each of the liquid filling components (73).

8. The nuclear magnetic resonance tube cleaning apparatus as described in claim 3, characterized in that, The NMR tube cleaning device further includes a drying component for drying the residual liquid inside the NMR tube (2) and the liquid guide tube (3) after cleaning; the drying component includes: A heating element (31) and a second gas source (32) are provided. The two ends of the heating element (31) are connected to the second gas source (32) and the transfer valve (8) respectively. The transfer valve (8) is selectively connected to the heating element (31). The heating element (31) is used to heat the gas supplied by the second gas source (32) and to make the heated gas flow into the liquid guide tube (3) to dry the residual liquid in the nuclear magnetic tube (2) and the liquid guide tube (3). When the residual liquid is dried, the liquid guide tube (3) selectively moves upward back to the initial position. The fifth valve (33) and the second exhaust component (34) are respectively connected to the nuclear magnetic tube (2) and the second exhaust component (34) to discharge the heating gas used to dry the residual liquid in the nuclear magnetic tube (2) and the liquid guide tube (3).

9. A method for cleaning nuclear magnetic resonance tubes, characterized in that, The nuclear magnetic resonance tube cleaning apparatus based on any one of claims 1-8 includes the following steps: S1: The blowing assembly (5) fills the nuclear magnetic tube (2) with gas so that the residual liquid in the nuclear magnetic tube (2) is classified and flowed into the first return liquid assembly (6) through the liquid guide tube (3); S2: Then, the filling assembly (7) fills the cleaning solution into the liquid guide tube (3) so that the cleaning solution soaks the inner wall of the nuclear magnetic tube (2); S3: After soaking is completed, the air blowing component (5) is used to fill the nuclear magnetic tube (2) with gas so that the cleaning liquid flows through the liquid guide tube (3) to the outside of the nuclear magnetic tube (2) and the cleaning liquid is sorted and recycled.

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