A method for controlling residual oxygen amount in an ampoule liquid infusion process

Abstract

The present application relates to a kind of ampoule liquid infusion process residual oxygen amount control method, the method includes the following steps, first, by the first nitrogen filling needle of bevel structure is injected into nitrogen into empty ampoule, nitrogen flows to the first nitrogen filling needle by nitrogen pipeline, flowmeter and switch valve are sequentially arranged on nitrogen pipeline along the flow direction of nitrogen;Second, by liquid injection needle is injected into liquid into empty ampoule;Third, by the second nitrogen filling needle is injected into nitrogen into ampoule, the gas outlet of second nitrogen filling needle is provided with flower mouth structure, flower mouth structure includes multiple resistance petals being spaced apart along the circumference, there is airflow passage between adjacent two resistance petals in circumference and between the bottom of each group of gas petal;Fourth, pull out the second nitrogen filling needle, ampoule is sealed.The present application provides a kind of ampoule liquid infusion process residual oxygen amount control method, which can effectively reduce the residual oxygen amount in ampoule during liquid infusion process.

Description

Technical Field

[0001] This invention relates to the field of tablet manufacturing technology, and in particular to a method for controlling residual oxygen levels during the ampoule filling process. Background Technology

[0002] During the filling process of ampoules, the control of residual oxygen level has a significant impact on the quality and stability of the medicine.

[0003] The traditional ampoule filling process is as follows: First, nitrogen gas is injected into the empty ampoule through a beveled nitrogen-filling needle, called primary nitrogen filling, to remove oxygen from the empty ampoule; second, medication is injected into the empty ampoule through the injection needle; third, nitrogen gas is injected a second time through the beveled nitrogen-filling needle into the upper part of the medication in the ampoule, called secondary nitrogen filling, to reduce oxygen mixed into the ampoule during medication injection; fourth, the nitrogen-filling needle is removed, and the top of the ampoule is sealed.

[0004] Existing technology testing revealed that using current processes to fill and seal ampoules does not effectively control residual oxygen levels, with a residual oxygen concentration remaining around 2%, which is not particularly conducive to long-term stable storage of medications. Through multiple experiments and theoretical analyses, we found that the shape of the needle used for primary and secondary nitrogen filling, the height of the needle insertion into the ampoule, the filling speed of the medication, the sealing position of the ampoule, and the flow path of nitrogen are all major factors affecting residual oxygen levels. Summary of the Invention

[0005] The purpose of this invention is to provide a method for controlling residual oxygen content in ampoules during the ampoule filling process, which can effectively reduce the residual oxygen content in the ampoule during the filling process.

[0006] To solve the above-mentioned technical problems, the technical solution of the present invention for controlling the residual oxygen content during the ampoule filling process is as follows:

[0007] A method for controlling residual oxygen content during ampoule filling includes the following steps: First, nitrogen gas is injected into an empty ampoule through a first nitrogen-filling needle with a beveled opening to achieve primary nitrogen filling. The nitrogen gas flows through a nitrogen pipeline to the first nitrogen-filling needle, and a flow meter and a switch valve are sequentially arranged along the flow direction of the nitrogen gas in the nitrogen pipeline. Second, liquid medicine is injected into the empty ampoule through an injection needle. Third, nitrogen gas is injected into the ampoule through a second nitrogen-filling needle to achieve secondary nitrogen filling. The outlet of the second nitrogen-filling needle has a perforated structure, which includes multiple circumferentially spaced air-blocking valves. There are airflow channels between adjacent air-blocking valves and between the bottoms of each group of valves. Fourth, the second nitrogen-filling needle is removed to seal the ampoule.

[0008] Furthermore, the second nitrogen filling needle includes a second needle tube, the upper end of each gas-blocking valve is hinged to the bottom of the second needle tube, and an elastic ring is attached to the outer periphery of each gas-blocking valve to force the lower ends of each gas-blocking valve to move closer to each other. A drive sleeve is mounted on the outer periphery of the second needle tube in a vertical direction, and the drive sleeve is driven by a drive sleeve drive mechanism. The lower end of the drive sleeve is provided with a gas-blocking valve pull rope that is connected to the bottom of the outer periphery of each gas-blocking valve.

[0009] Furthermore, each air-blocking valve has an elastic ring positioning groove along its outer periphery, with the elastic ring positioned in the corresponding elastic ring positioning groove.

[0010] Furthermore, the elastic ring is bonded to the wall of the elastic ring positioning groove.

[0011] Furthermore, the drive sleeve drive mechanism includes a left drive roller and a right drive roller located on the left and right sides of the drive sleeve. The left drive roller is driven by a left motor, and the right drive roller is driven by a right motor. The outer periphery of the left drive roller and the right drive roller has an arc-shaped groove that matches the outer periphery of the drive sleeve. The drive sleeve drive mechanism also includes a power component for driving the left drive roller and the right drive roller to move relative to each other so that the arc-shaped groove contacts the outer periphery of the drive sleeve.

[0012] Furthermore, the ampoule has a capacity of 1 ml, the first and second nitrogen filling needles are 0.7 cm above the bottom of the ampoule, the nitrogen flow rate during the first and second nitrogen filling is 7 L / min, the injection speed of the injection needle into the ampoule is 550 ampoules / min, and in the fourth step, the sealing position is 4.5 cm above the bottom of the ampoule.

[0013] Furthermore, the ampoule has a capacity of 2ml, the first and second nitrogen filling needles are 2cm above the bottom of the ampoule, the nitrogen flow rate during the first and second nitrogen filling is 8L / min, the injection speed of the injection needle into the ampoule is 500 ampoules / minute, and in the fourth step, the sealing position is 5.5cm above the bottom of the ampoule.

[0014] Furthermore, the ampoule has a capacity of 5ml, the first and second nitrogen filling needles are 2cm above the bottom of the ampoule, the nitrogen flow rate during the first and second nitrogen filling is 10L / min, the injection speed of the injection needle into the ampoule is 350 ampoules / minute, and in the fourth step, the sealing position is 7cm above the bottom of the ampoule.

[0015] Furthermore, the ampoule has a capacity of 10ml, the first and second nitrogen filling needles are 3.5cm above the bottom of the ampoule, the nitrogen flow rate during the first and second nitrogen filling is 13L / min, the injection speed of the injection needle into the ampoule is 300 ampoules / minute, and in the fourth step, the sealing position is 8cm above the bottom of the ampoule.

[0016] Furthermore, the ampoule has a capacity of 20ml, the first and second nitrogen filling needles are 4cm above the bottom of the ampoule, the nitrogen flow rate during the first and second nitrogen filling is 15L / min, the injection speed of the injection needle into the ampoule is 200 ampoules / minute, and in the fourth step, the sealing position is 11cm above the bottom of the ampoule.

[0017] The beneficial effects of this invention are as follows: In the first nitrogen filling, there is no medicine in the ampoule. Therefore, a first nitrogen filling needle with a beveled opening is used. The beveled opening has a large air outlet area, which can achieve rapid nitrogen filling of the ampoule, so that the original oxygen in the ampoule is quickly and completely squeezed out. At the same time, the nitrogen gas first passes through a flow meter and then through a switch valve. When the nitrogen filling value reaches the closing valve, the ampoule can obtain an accurate nitrogen filling amount. In the second nitrogen filling, since there is already medicine in the ampoule, using a nitrogen filling needle with a beveled opening can easily cause liquid level fluctuations during the nitrogen filling process, resulting in changes in the oxygen content in the ampoule. Therefore, a second nitrogen filling needle with a scalloped opening is used, which makes the nitrogen gas diffusion more uniform, thereby ensuring that the oxygen mixed in by the ampoule is fully squeezed out, and ultimately effectively controlling the residual oxygen content in the ampoule. Attached Figure Description

[0018] The above and other objects, features, and advantages of this disclosure will become readily apparent from the following detailed description of exemplary embodiments with reference to the accompanying drawings. In the drawings, several embodiments of this disclosure are illustrated by way of example and not limitation, and like or corresponding reference numerals denote like or corresponding portions, wherein:

[0019] Figure 1 This is a flowchart of the ampoule filling process in this invention;

[0020] Figure 2 yes Figure 1 middle Figure 1 A schematic diagram showing the interaction between the second nitrogen-filling needle and the drive mechanism of the drive sleeve;

[0021] Figure 3 yes Figure 2 Top view;

[0022] Figure 4 yes Figure 2 Schematic diagram of the drive mechanism of the middle drive sleeve;

[0023] Figure 5 yes Figure 2 Enlarged view of point A in the image;

[0024] Figure 6 yes Figure 5A schematic diagram showing the state after the middle drive sleeve moves upward and the lower ends of each air-blocking valve move backward and open; 1. Conveying mechanism; 2. Slanted opening structure; 3. Ampoule; 4. First nitrogen-filling needle; 5. Medicine liquid; 6. Injection needle; 7. Second nitrogen-filling needle; 8. Drive sleeve; 9. Right side motor; 10. Left side drive roller; 11. Drive sleeve drive mechanism; 12. Floral opening structure; 13. Second needle tube; 14. First drive cylinder; 15. Second drive cylinder; 16. First hinge arm; 17. Second hinge arm; 18. Right side drive roller; 19. Left side motor; 20. Air-blocking valve pull rope; 21. Air-blocking valve; 22. Airflow channel; 23. Elastic ring; 24. Hinge structure. Detailed Implementation

[0025] To facilitate understanding of the present invention, a more detailed description is provided below with reference to the accompanying drawings and specific embodiments. Preferred embodiments of the invention are shown in the drawings. However, the invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of the invention.

[0026] It should be noted that, unless otherwise defined, all technical and scientific terms used in this specification have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to limit the invention.

[0027] An example of implementing a method for controlling residual oxygen levels during ampoule filling in this invention is as follows: Figures 1-6 As shown:

[0028] The method includes the following steps: First, nitrogen gas is injected into an empty ampoule 3 through the first nitrogen-filling needle 4 of the oblique structure 2 to achieve primary nitrogen filling. The nitrogen gas flows to the first nitrogen-filling needle through the first nitrogen gas pipeline. A first flow meter and a first switching valve are arranged sequentially along the flow direction of the nitrogen gas on the nitrogen gas pipeline. Second, liquid medicine 5 is injected into the empty ampoule 3 through the liquid injection needle 6. Third, nitrogen gas is injected into the ampoule through the second nitrogen-filling needle 7 to achieve secondary nitrogen filling. The nitrogen gas flows to the second nitrogen-filling needle through the second nitrogen gas pipeline. A second flow meter and a second switching valve are arranged sequentially along the flow direction of the nitrogen gas on the second nitrogen gas channel. The outlet of the second nitrogen-filling needle is provided with a flower-shaped structure 12. The flower-shaped structure 12 includes multiple circumferentially spaced air-blocking petals 21. There are airflow channels 22 between two adjacent air-blocking petals in the circumferential direction and between the bottoms of each group of petals. Fourth, the second nitrogen-filling needle is pulled out to seal the ampoule.

[0029] The first nitrogen-filling needle 4 with the oblique opening structure is existing technology and will not be described in detail here.

[0030] The second nitrogen-filling needle 7 includes a second needle tube 13. The upper ends of each gas-blocking valve are hinged to the bottom of the second needle tube via a hinge structure 24. In this embodiment, the hinge structure is a hinge. Each gas-blocking valve is surrounded by an elastic ring 23 for forcing the lower ends of each gas-blocking valve to move closer together. A drive sleeve 8 is mounted on the outer periphery of the second needle tube in a vertical direction. The drive sleeve 8 is driven by a drive sleeve drive mechanism 11. The lower end of the drive sleeve 8 is provided with gas-blocking valve pull ropes 20, which are respectively connected to the bottom of the outer periphery of each gas-blocking valve. In this embodiment, there are four gas-blocking valves, so there are also four gas-blocking valve pull ropes 20. Each gas-blocking valve pull rope is connected to a corresponding gas-blocking valve. The gas-blocking valve pull rope is located on the outside of the corresponding gas-blocking valve. The upper end of the gas-blocking valve pull rope is connected to the bottom of the drive sleeve 8, and the lower end of the gas-blocking valve pull rope 20 is connected to the outer side of the lower end of the corresponding gas-blocking valve 21.

[0031] When the drive sleeve 8 is positioned relatively low, under the clamping action of the elastic ring 23, the lower ends of each air-blocking valve move closer together, and the airflow channel narrows. When the drive sleeve moves upward, the drive sleeve pulls the lower end of the corresponding air-blocking valve in opposite directions through the air-blocking valve pull rope, and the airflow channel widens.

[0032] In this embodiment, each air-blocking valve is provided with an elastic ring positioning groove along its outer periphery, and the elastic ring 23 is located in the corresponding elastic ring positioning groove. The elastic ring 23 is bonded to the groove wall of the elastic ring positioning groove.

[0033] The drive sleeve drive mechanism includes a left drive roller 10 and a right drive roller 18 located on the left and right sides of the drive sleeve. The left drive roller 10 is driven by a left motor 19, and the right drive roller 18 is driven by a right motor 9. The outer periphery of the left and right drive rollers has an arc-shaped groove adapted to the outer periphery of the drive sleeve. The drive sleeve drive mechanism also includes a power component for driving the left and right drive rollers to move relative to each other to achieve contact between the arc-shaped groove and the outer periphery of the drive sleeve. In this embodiment, the left motor is located in front of the left drive roller, and the right motor is located behind the right drive roller. The left and right motors are diagonally positioned, which helps to ensure the stability of the entire structure.

[0034] The two ends of the right drive roller are rotatably mounted on two front-to-back second hinge arms 17, and the two ends of the left drive roller are rotatably mounted on two front-to-back first hinge arms 16. The front first hinge arm 16 is hinged to the front second hinge arm 17; the rear first hinge arm 16 is hinged to the rear second hinge arm 17. The drive sleeve drive mechanism also includes a second drive cylinder 15 corresponding to each of the first hinge arms and a first drive cylinder 14 corresponding to each of the second hinge arms. When the piston rods of the first drive cylinder 14 and the second drive cylinder 15 extend, the first hinge arm 16 and the second hinge arm 17 rotate, and the left drive roller 10 and the right drive roller 18 swing relative to each other. These left and right drive rollers can clamp the drive sleeve. The left motor 19 drives the left drive roller 10 to rotate, and the right motor 9 drives the right drive roller 18 to rotate. The left and right drive rollers rub and roll with the drive sleeve, which can move the drive sleeve 8 up and down. When the piston rods of the first drive cylinder 14 and the second drive cylinder 15 retract, the left and right drive rollers swing in opposite directions, which can release the clamping effect on the drive sleeve. The first drive cylinder and the second drive cylinder are mounted on corresponding fixed brackets (not shown in the figure), and the hinge shafts of the first hinge arm and the second hinge arm are also set on corresponding fixed brackets.

[0035] When the ampoule has a capacity of 1 ml, the distance between the first and second nitrogen filling needles and the bottom of the ampoule is 0.7 cm. The nitrogen flow rate during the first and second nitrogen filling is 7 L / min. The injection speed of the injection needle into the ampoule is 550 ampoules / min. In the fourth step, the distance between the sealing position and the bottom of the ampoule is 4.5 cm.

[0036] When the ampoule has a capacity of 2ml, the first and second nitrogen filling needles are 2cm away from the bottom of the ampoule. The nitrogen flow rate during the first and second nitrogen filling is 8L / min. The injection speed of the injection needle into the ampoule is 500 ampoules / minute. In the fourth step, the sealing position is 5.5cm away from the bottom of the ampoule.

[0037] When the ampoule has a capacity of 5ml, the distance between the first and second nitrogen filling needles and the bottom of the ampoule is 2cm. The nitrogen flow rate during the first and second nitrogen filling is 10L / min. The injection speed of the injection needle into the ampoule is 350 ampoules / minute. In the fourth step, the distance between the sealing position and the bottom of the ampoule is 7cm.

[0038] When the ampoule has a capacity of 10ml, the distance between the first and second nitrogen filling needles and the bottom of the ampoule is 3.5cm. The nitrogen flow rate during the first and second nitrogen filling is 13L / min. The injection speed of the injection needle into the ampoule is 300 ampoules / minute. In the fourth step, the distance between the sealing position and the bottom of the ampoule is 8cm.

[0039] When the ampoule has a capacity of 20ml, the first and second nitrogen filling needles are 4cm away from the bottom of the ampoule. The nitrogen flow rate during the first and second nitrogen filling is 15L / min. The injection speed of the injection needle into the ampoule is 200 ampoules / minute. In the fourth step, the sealing position is 11cm away from the bottom of the ampoule.

[0040] Because the height of the second nitrogen-filling needle from the bottom of the ampoule varies depending on its capacity, the corresponding nitrogen flow rate also differs. During the second nitrogen filling, the ampoule already contains medication. If the size of the airflow channel on the spout structure cannot be adjusted, excessively high airflow velocity may cause fluctuations in the medication. Therefore, when the height of the spout structure relative to the medication level is small, the drive sleeve moves upward, widening the airflow channel and reducing the airflow velocity to prevent excessive velocity and surface fluctuations. When the height of the spout structure relative to the medication level is large, the drive sleeve moves downward, narrowing the airflow channel and appropriately increasing the airflow velocity, allowing nitrogen to quickly reach the medication level and expel oxygen from the ampoule. In this invention, the drive sleeve drives the gas-blocking valve to swing around the hinge axis of the hinge structure, thereby adjusting the airflow channel size. This makes the second nitrogen-filling needle suitable for secondary nitrogen filling of various ampoule sizes, offering good versatility.

[0041] To verify the technical effectiveness of the corresponding technical solution of this invention, the following testing method was adopted: Water for injection was added to the preparation vessel, the solution temperature was set to approximately 30°C, and the solution was filtered using 0.45μm and 0.22μm polyethersulfone membranes before the second step of drug filling. Throughout the filling process, the ambient temperature was maintained between 20°C and 25°C, and the humidity was controlled between 40% and 60% to further improve the accuracy of residual oxygen control. High-purity nitrogen (purity ≥99.99%) was used to ensure the quality of the injected gas. 200 vials were filled according to each condition in the table, and 6 vials were randomly selected for testing, as shown in the figure below:

[0042]

[0043]

[0044] In the diagram above, the beveled tip indicates a needle used for nitrogen filling, while the swivel tip indicates a needle used for nitrogen filling. The fifth column from left to right shows the height of the filling needle from the bottom of the ampoule during the first and second nitrogen filling processes. The sixth column from left to right shows the nitrogen flow rate during the first and second nitrogen filling processes. The seventh column from left to right shows the sequence of the switching valve and flow meter in the nitrogen delivery path. From the diagram above, it is clear that:

[0045] When the ampoule has a capacity of 1 ml, the distance between the first and second nitrogen-filling needles and the bottom of the ampoule is 0.7 cm. The nitrogen flow rate during the first and second nitrogen filling is 7 L / min. The injection rate of the injection needle into the ampoule is 550 ampoules / minute. In the fourth step, the distance between the sealing position and the bottom of the ampoule is 4.5 cm. This method results in the lowest residual oxygen content in the ampoule and is the optimal solution.

[0046] When the ampoule has a capacity of 2ml, the distance between the first and second nitrogen-filling needles and the bottom of the ampoule is 2cm. The nitrogen flow rate during the first and second nitrogen filling is 8L / min. The injection rate of the injection needle into the ampoule is 500 ampoules / minute. In the fourth step, the distance between the sealing position and the bottom of the ampoule is 5.5cm. This method results in the lowest residual oxygen content in the ampoule and is the optimal solution.

[0047] When the ampoule has a capacity of 5ml, the distance between the first and second nitrogen-filling needles and the bottom of the ampoule is 2cm. The nitrogen flow rate during the first and second nitrogen filling is 10L / min. The injection rate of the injection needle into the ampoule is 350 ampoules / minute. In the fourth step, the distance between the sealing position and the bottom of the ampoule is 7cm. This method results in the lowest residual oxygen content inside the ampoule and is the optimal solution.

[0048] When the ampoule has a capacity of 10ml, the distance between the first and second nitrogen-filling needles and the bottom of the ampoule is 3.5cm. The nitrogen flow rate during the first and second nitrogen filling is 13L / min. The injection rate of the injection needle into the ampoule is 300 ampoules / minute. In the fourth step, the distance between the sealing position and the bottom of the ampoule is 8cm. This method results in the lowest residual oxygen content inside the ampoule and is the optimal solution.

[0049] When the ampoule has a capacity of 20ml, the distance between the first and second nitrogen filling needles and the bottom of the ampoule is 4cm. The nitrogen flow rate during the first and second nitrogen filling is 15L / min. The injection rate of the injection needle into the ampoule is 200 ampoules / minute. In the fourth step, the distance between the sealing position and the bottom of the ampoule is 11cm. This method results in the lowest residual oxygen content in the ampoule and is the optimal solution.

[0050] The filling sequence of the present invention is as follows Figure 1 As shown, ampoules of the corresponding specifications are moved stepwise from left to right by a conveying mechanism. When the ampoule moves to the underside of the first nitrogen-filling needle, the first nitrogen-filling needle descends and extends into the ampoule to complete the first nitrogen filling. Subsequently, when the ampoule is moved from left to right by the conveying mechanism to the underside of the liquid injection needle, the liquid injection needle descends and extends into the ampoule to inject liquid. Then, the ampoule is moved from left to right by the conveying mechanism to the underside of the second nitrogen-filling needle, the second nitrogen-filling needle descends and extends into the ampoule to complete the second nitrogen filling. Afterward, the conveying mechanism continues to move to the right with the ampoule to perform a flame sealing operation.

[0051] In the foregoing description of this specification, unless otherwise expressly specified and limited, the terms "fixed," "installed," "connected," or "linked" should be interpreted broadly. For example, the term "linked" can refer to a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; or it can refer to the internal communication of two components or the interaction between two components. Therefore, unless otherwise expressly limited in this specification, those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0052] Based on the above description in this specification, those skilled in the art will also understand that terms used, such as "upper," "lower," "front," "rear," "left," "right," "length," "width," "thickness," "vertical," "horizontal," "top," "bottom," "inner," "outer," "axial," "radial," "circumferential," "center," "longitudinal," "transverse," "clockwise," or "counterclockwise," are terms indicating orientation or positional relationships based on the orientation or positional relationships shown in the accompanying drawings of this specification. They are only for the purpose of facilitating the explanation of the present invention and simplifying the description, and do not imply that the devices or elements involved must have the specific orientation, or be constructed and operated in a specific orientation. Therefore, the above-mentioned orientation or positional relationship terms should not be understood or interpreted as limitations on the present invention.

[0053] Furthermore, the terms "first" or "second," etc., used in this specification to refer to numbers or ordinal numbers are for descriptive purposes only and should not be construed as indicating, explicitly or implicitly, relative importance or specifying the number of indicated technical features. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this specification, "a plurality of" means at least two, such as two, three, or more, unless otherwise explicitly specified.

[0054] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for controlling residual oxygen levels during ampoule filling, characterized in that: The method includes the following steps: First, nitrogen gas is injected into an empty ampoule through a first nitrogen-filling needle with a beveled opening to achieve primary nitrogen filling. The nitrogen gas flows through a nitrogen pipeline to the first nitrogen-filling needle, and a flow meter and a switch valve are arranged sequentially along the flow direction of the nitrogen gas on the nitrogen pipeline. Second, liquid medicine is injected into the empty ampoule through an injection needle. Third, nitrogen gas is injected into the ampoule through a second nitrogen-filling needle to achieve secondary nitrogen filling. The outlet of the second nitrogen-filling needle has a spout structure, which includes multiple circumferentially spaced air-blocking flaps. There are airflow channels between adjacent air-blocking flaps and between the bottoms of each air-blocking flap. Fourth, the second nitrogen-filling needle is removed to seal the ampoule.

2. The residual oxygen control method according to claim 1, characterized in that: The second nitrogen-filling needle includes a second needle tube. The upper end of each gas-blocking valve is hinged to the bottom of the second needle tube. Each gas-blocking valve has an elastic ring around its outer periphery to force the lower ends of each gas-blocking valve to move closer together. A drive sleeve is mounted on the outer periphery of the second needle tube in a vertical direction. The drive sleeve is driven by a drive sleeve drive mechanism. The lower end of the drive sleeve is provided with a gas-blocking valve pull rope that is connected to the bottom of the outer periphery of each gas-blocking valve.

3. The residual oxygen control method according to claim 2, characterized in that: Each air-blocking valve has an elastic ring positioning groove along its outer periphery, and the elastic ring is positioned in the corresponding elastic ring positioning groove.

4. The residual oxygen control method according to claim 3, characterized in that: The elastic ring is bonded to the wall of the elastic ring positioning groove.

5. The residual oxygen control method according to claim 2, characterized in that: The drive sleeve drive mechanism includes a left drive roller and a right drive roller located on the left and right sides of the drive sleeve. The left drive roller is driven by a left motor and the right drive roller is driven by a right motor. The outer periphery of the left drive roller and the right drive roller has an arc-shaped groove that matches the outer periphery of the drive sleeve. The drive sleeve drive mechanism also includes a power component for driving the left drive roller and the right drive roller to move relative to each other so that the arc-shaped groove contacts the outer periphery of the drive sleeve.

6. The residual oxygen control method according to any one of claims 1 to 5, characterized in that: The ampoule has a capacity of 1 ml. The first and second nitrogen filling needles are 0.7 cm above the bottom of the ampoule. The nitrogen flow rate during the first and second nitrogen filling is 7 L / min. The injection speed of the injection needle into the ampoule is 550 ampoules / min. In the fourth step, the sealing position is 4.5 cm above the bottom of the ampoule.

7. The residual oxygen control method according to any one of claims 1 to 5, characterized in that: The ampoule has a capacity of 2ml. The first and second nitrogen filling needles are 2cm above the bottom of the ampoule. The nitrogen flow rate during the first and second nitrogen filling is 8L / min. The injection speed of the injection needle into the ampoule is 500 ampoules / minute. In the fourth step, the sealing position is 5.5cm above the bottom of the ampoule.

8. The residual oxygen control method according to any one of claims 1 to 5, characterized in that: The ampoule has a capacity of 5ml. The first and second nitrogen filling needles are 2cm away from the bottom of the ampoule. The nitrogen flow rate during the first and second nitrogen filling is 10L / min. The injection speed of the injection needle into the ampoule is 350 ampoules / minute. In the fourth step, the sealing position is 7cm away from the bottom of the ampoule.

9. The residual oxygen control method according to any one of claims 1 to 5, characterized in that: The ampoule has a capacity of 10ml. The first and second nitrogen filling needles are 3.5cm above the bottom of the ampoule. The nitrogen flow rate during the first and second nitrogen filling is 13L / min. The injection speed of the injection needle into the ampoule is 300 ampoules / minute. In the fourth step, the sealing position is 8cm above the bottom of the ampoule.

10. The residual oxygen control method according to any one of claims 1 to 5, characterized in that: The ampoule has a capacity of 20ml. The first and second nitrogen filling needles are 4cm away from the bottom of the ampoule. The nitrogen flow rate during the first and second nitrogen filling is 15L / min. The injection speed of the injection needle into the ampoule is 200 ampoules / minute. In the fourth step, the sealing position is 11cm away from the bottom of the ampoule.

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