A standard gas configuration feed liquid adding device and an adding method thereof

Abstract

The application discloses a standard gas configuration raw material liquid adding device, which comprises a high-pressure steel cylinder, a flowmeter, a first three-way valve, a second three-way valve, a vacuum pump and an annular heating pipeline, a pressure reducing valve is arranged on the gas outlet pipeline of the high-pressure steel cylinder, the gas outlet pipeline of the high-pressure steel cylinder is connected with one port of the first three-way valve, the second port of the first three-way valve is connected with the gas inlet of the vacuum pump, the third port of the first three-way valve is connected with the hose interface end of one end of the cross pipe of the second three-way valve, the hose interface end of the other end of the cross pipe of the second three-way valve is connected with one end of the annular heating pipeline through a fixed-length hose, and the annular heating pipeline is connected with the steel cylinder joint of a sample steel cylinder. The three-stage heating device can effectively solve the liquid gasification problem, the annular pipeline is designed to heat, the un-gasified liquid is effectively retained in the annular pipeline and is heated and gasified, and the vacuum pump cleaning pipeline can solve the influence of impurities in residual air in the pipeline on the finished gas.

Description

Technical Field

[0001] This invention relates to the field of liquid quantitative addition technology, and in particular to a raw material liquid addition device and method with standard gas configuration. Background Technology

[0002] In gas preparation, the addition of liquids requires transferring them to gas cylinders in specific quantities according to a set procedure. Due to differences in the boiling points, adsorption capacities, and other physicochemical properties of the raw materials, varying degrees of mass loss occur during this transfer process. This means that the required amount of raw material may not completely enter the standard gas cylinder, leading to instability and deviations in the preparation results. Therefore, designing a liquid addition device for more efficient liquid transfer is a crucial technology for preventing liquid loss during gas preparation. Summary of the Invention

[0003] This invention aims to at least partially solve one of the technical problems in related technologies. Therefore, one objective of this invention is to provide a raw material liquid addition device and method for standard gas preparation, which solves the problem of instability in the preparation results caused by liquid loss during liquid addition in the gas preparation process.

[0004] According to the present invention, a raw material liquid addition device with standard gas configuration includes a high-pressure cylinder, a flow meter, a first three-way valve, a second three-way valve, a vacuum pump, and an annular heating pipe. The outlet pipe of the high-pressure cylinder is equipped with a pressure reducing valve. The outlet pipe of the high-pressure cylinder is connected to one port of the first three-way valve via a fixed-length hose. The second port of the first three-way valve is connected to the inlet of the vacuum pump via a fixed-length hose, and a vacuum switch is provided on this fixed-length hose. The second three-way valve includes a horizontally placed horizontal pipe and a vertical pipe perpendicular to the middle of the horizontal pipe. Both ends of the horizontal pipe are hose interface ends, and manual valves are provided near both ends. A manual valve is also provided on the vertical pipe. The third port of the first three-way valve is connected to the hose interface end of one end of the horizontal pipe of the second three-way valve via a fixed-length hose. The hose interface end of the other end of the horizontal pipe of the second three-way valve is connected to one end of the annular heating pipe via a fixed-length hose. The other end of the annular heating pipe is connected to the cylinder connector of a sample cylinder via a fixed-length hose.

[0005] The first three-way valve, the second three-way valve, and the annular heating pipe are located in the main heating zone, and the second three-way valve is located in the secondary heating zone, which is inside the main heating zone.

[0006] In some embodiments of the present invention, the high-pressure cylinder is provided with a heating device, which can heat the high-pressure cylinder to 60°C.

[0007] In other embodiments of the present invention, the heating temperature range of the main heating zone is 25-80°C, and the heating temperature range of the secondary heating zone is 80-120°C.

[0008] In other embodiments of the present invention, an electromagnetic coil wound in a spiral shape is wound on the annular heating pipe, and the annular heating pipe is a metal pipe.

[0009] A method for adding a raw material liquid prepared with a standard gas, comprising using the aforementioned raw material liquid adding device prepared with a standard gas, and the adding steps are as follows:

[0010] S1: Close the pressure reducing valve and the valve on the cylinder connector of the sample cylinder, open the three valves on the first three-way valve, open the manual valves at both ends of the horizontal pipe on the second three-way valve and close the manual valve on the vertical pipe.

[0011] S2: Heat the temperature inside the high-pressure cylinder to 50-60℃ and the main heating zone to 70-80℃ until the temperature stabilizes;

[0012] S3: Turn on the vacuum switch and start the vacuum pump to evacuate the vacuum. After evacuating for a period of time, turn off the vacuum switch in time, open the pressure reducing valve, and exhaust the gas into the pipeline through the high-pressure cylinder so that the pressure of the high-purity gas in the pipeline is 0.5MPa.

[0013] S4: Repeat step S3 at least 10 times to completely fill the pipeline with high-purity gas. At this point, the vacuum switch is turned off.

[0014] S5: Close the manual valves at both ends of the horizontal tube of the second three-way valve, then open the manual valve on the vertical tube. Inject a metered amount of raw material liquid into the second three-way valve through the injection port of the vertical tube using a metering syringe. Then close the manual valve on the vertical tube. The auxiliary heating zone heats the second three-way valve to 120°C. Then, open the manual valves at both ends of the horizontal tube of the second three-way valve and close the flow meter.

[0015] S6: Adjust the pressure of the pressure reducing valve to 0.6MPa, open valve 71 on the cylinder connector of the sample cylinder, and open the flow meter to adjust the flow rate to 0.5 liters / minute;

[0016] S7: When the pressure of the sample cylinder reaches the secondary pressure of 0.6MPa, the flow rate of the flow meter will approach 0. Close the valve on the sample cylinder, close the flow meter, close the pressure reducing valve, disassemble the pipeline, and the addition is complete.

[0017] In other embodiments of the present invention, the annular heating pipe is heated by an electromagnetic coil. If the annular heating pipe needs to be heated to a temperature higher than that of the main heating zone, it is necessary to first heat it by the electromagnetic coil and maintain the heating temperature for 10 minutes.

[0018] In some other embodiments of the present invention, when adding a quantitative amount of raw material liquid into the second three-way valve in step S5, heat-resistant gloves are worn.

[0019] In other embodiments of the present invention, the heating temperatures of the main heating zone, the secondary heating zone, and the annular heating pipe 6 are adjusted according to the vaporization temperature of the added liquid and the injection volume.

[0020] In this invention, a three-stage heating device is designed during the liquid transfer process, which effectively solves the problem of liquid vaporization and makes up for the defect that the liquid cannot be completely added to the sample bottle due to the liquid adhering to the pipeline, interface, etc.

[0021] Because the flow rate of liquid is slower than that of gas, the ring pipeline design effectively retains the unvaporized liquid in the ring pipeline, and the vaporized raw material enters the sample cylinder along with the carrier gas.

[0022] Heating the high-pressure cylinder ensures that the carrier gas is at a high temperature during the filling process, preventing other heating areas from becoming ineffective due to excessively low carrier gas temperature.

[0023] Vacuum pumps can clean pipelines, which can solve the problem of impurities in the residual air affecting the finished product gas, and can also extract residual raw materials to avoid harm to the human body. Attached Figure Description

[0024] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used in conjunction with embodiments of the invention to explain the invention and do not constitute a limitation thereof. In the drawings:

[0025] Figure 1 This is a schematic diagram of a raw material liquid addition device with standard gas configuration proposed in this invention.

[0026] Figure 2 This is a schematic diagram of the structure of the second three-way valve proposed in this invention.

[0027] Figure 3 This is a schematic diagram of a partial segment of the annular heating pipe proposed in this invention.

[0028] In the diagram: 1. High-pressure gas cylinder; 11. Pressure reducing valve; 2. Flow meter; 3. First three-way valve; 4. Vacuum pump; 41. Vacuum switch; 5. Second three-way valve; 51. Manual valve; 6. Annular heating pipe; 61. Electromagnetic coil; 7. Sample gas cylinder; 71. Valve on gas cylinder connector. Detailed Implementation

[0029] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0030] This invention proposes a standard gas-configured raw material liquid addition device, comprising a high-pressure cylinder 1, a flow meter 2, a first three-way valve 3, a second three-way valve 5, a vacuum pump 4, and an annular heating pipe 6. The outlet pipe of the high-pressure cylinder 1 is equipped with a pressure reducing valve 11. The outlet pipe of the high-pressure cylinder 1 is connected to one port of the first three-way valve 3 via a fixed-length flexible hose. The second port of the first three-way valve 3 is connected to the inlet of the vacuum pump 4 via a fixed-length flexible hose, and a vacuum switch 41 is provided on this fixed-length flexible hose. The second three-way valve 5 includes a... A horizontally placed horizontal tube and a vertical tube perpendicular to the middle of the horizontal tube. Both ends of the horizontal tube are hose interface ends and manual valves 51 are provided near the ends. The vertical tube is also provided with manual valves 51. The third port of the first three-way valve 3 is connected to the hose interface end of one end of the horizontal tube of the second three-way valve 5 through a fixed-length hose. The hose interface end of the other end of the horizontal tube of the second three-way valve 5 is connected to one end of the annular heating pipe 6 through a fixed-length hose. The other end of the annular heating pipe 6 is connected to the cylinder connector of the sample cylinder 7 through a fixed-length hose.

[0031] The first three-way valve 3, the second three-way valve 5, and the annular heating pipe 6 are located in the main heating zone, and the second three-way valve 5 is located in the auxiliary heating zone, which is inside the main heating zone.

[0032] The connecting hoses are high-temperature resistant (they will not be damaged at 100℃). The main heating zone is a heating chamber, while the auxiliary heating zone is a smaller heating chamber within the main heating zone. The multi-section fixed-length hose connection is designed to facilitate determining the vacuum pump's evacuation time for each cycle.

[0033] The gas inside high-pressure cylinder 1 is sufficient to complete at least one liquid refill.

[0034] The high-pressure cylinder 1 is equipped with a heating device that can heat the high-pressure cylinder 1 to 60°C.

[0035] The main heating zone has a heating temperature range of 25-80℃, and the auxiliary heating zone has a heating temperature range of 80-120℃.

[0036] A three-stage heating system was designed for the liquid transfer process to effectively solve the problem of liquid vaporization and compensate for the incomplete addition to the sample vial caused by liquid adhesion to pipelines and interfaces. The first stage of heating is the main heating, providing a high-temperature environment for the high-pressure nitrogen and the entire equipment. The second stage of heating is high-temperature heating at the injection port, i.e., heating via the second three-way valve 5, providing specific heating temperatures for different liquid raw materials. The third stage of heating occurs at the annular pipeline to prevent liquid condensation and ensure that the raw material entering the sample cylinder 7 is in a gaseous state.

[0037] A spiral electromagnetic coil 61 is wound around the annular heating pipe 6, which is a metal pipe. The heating temperature is achieved by adjusting the current flowing through the electromagnetic coil 61.

[0038] A method for adding a raw material liquid in a standard gas configuration, comprising the following steps:

[0039] S1: Close the pressure reducing valve 11 and the valve 71 on the cylinder connector of the sample cylinder 7, open the three valves on the first three-way valve 3, open the manual valves 51 at both ends of the horizontal pipe on the second three-way valve 5 and close the manual valve 51 on the vertical pipe.

[0040] S2: Heat the temperature inside high-pressure cylinder 1 to 50-60℃ and the main heating zone to 70-80℃ until the temperature stabilizes;

[0041] S3: Turn on vacuum switch 41 and turn on vacuum pump 4 to evacuate. After evacuating for a period of time, turn off vacuum switch 41 in time, open pressure reducing valve 11, and exhaust gas into the pipeline through high pressure cylinder 1 so that the pressure of high-purity gas in the pipeline is 0.5MPa.

[0042] S4: Repeat step S3 at least 10 times to completely fill the pipeline with high-purity gas. At this time, vacuum switch 41 is closed.

[0043] S5: Close the manual valves 51 at both ends of the horizontal tube of the second three-way valve 5, then open the manual valve 51 on the vertical tube. Inject a quantitative amount of raw material liquid into the second three-way valve 5 through the injection port of the vertical tube using a quantitative syringe. Then close the manual valve 51 on the vertical tube. The auxiliary heating zone heats the second three-way valve 5 to 120°C. Then, open the manual valves 51 at both ends of the horizontal tube of the second three-way valve 5 and close the flow meter 2.

[0044] S6: Adjust the pressure reducing valve 11 to a secondary pressure of 0.6 MPa, open valve 71 on the cylinder connector of sample cylinder 7, and open flow meter 2 to adjust the flow rate to 0.5 liters / minute (here, the flow rate can be adjusted according to the liquid vaporization temperature and liquid volume. If the vaporization temperature is high or the liquid content is high, the flow rate should be reduced).

[0045] S7: When the pressure of sample cylinder 7 reaches the secondary pressure of 0.6MPa, the flow rate of flow meter 2 tends to 0. Close valve 71 on sample cylinder 7, close flow meter 2, close pressure reducing valve 11, disassemble the pipeline, and the addition is completed.

[0046] The annular heating pipe 6 is heated by an electromagnetic coil 61. If the annular heating pipe 6 needs to be heated to a temperature higher than that of the main heating zone, it needs to be heated by the electromagnetic coil 61 and maintained at that temperature for 10 minutes. If the vaporization temperature is too high, the main heating zone temperature may not be able to vaporize properly, or condensation may occur. In this case, the annular heating pipe 6 is heated to prevent condensation.

[0047] When adding a measured amount of raw material liquid into the second three-way valve 5 in step S5, wear heat-resistant gloves. The operating environment temperature is generally high, and it is very easy to burn your hands.

[0048] The heating temperatures of the main heating zone, the secondary heating zone, and the annular heating pipe 6 are adjusted according to the vaporization temperature of the added liquid and the injection volume.

[0049] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A raw material liquid addition device with standard gas configuration, characterized in that: The system includes a high-pressure cylinder (1), a flow meter (2), a first three-way valve (3), a second three-way valve (5), a vacuum pump (4), and an annular heating pipe (6). A pressure reducing valve (11) is installed on the outlet pipe of the high-pressure cylinder (1). The outlet pipe of the high-pressure cylinder (1) is connected to one port of the first three-way valve (3) via a fixed-length flexible hose. The second port of the first three-way valve (3) is connected to the inlet of the vacuum pump (4) via a fixed-length flexible hose, and a vacuum switch (41) is installed on this fixed-length flexible hose. The second three-way valve (5) includes a horizontally placed crossbar. The pipe and the vertical pipe perpendicular to the middle position of the horizontal pipe, the two ends of the horizontal pipe are hose interface ends and manual valves (51) are provided near the two ends. The vertical pipe is also provided with manual valves (51). The third port of the first three-way valve (3) is connected to the hose interface end of the horizontal pipe of the second three-way valve (5) through a fixed length hose. The hose interface end of the other end of the horizontal pipe of the second three-way valve (5) is connected to one end of the annular heating pipe (6) through a fixed length hose. The other end of the annular heating pipe (6) is connected to the cylinder joint of the sample cylinder (7) through a fixed length hose. The first three-way valve (3), the second three-way valve (5) and the annular heating pipe (6) are located in the main heating zone, the second three-way valve (5) is located in the auxiliary heating zone, the auxiliary heating zone is inside the main heating zone, the high-pressure steel cylinder (1) is equipped with a heating device, the heating device can heat the high-pressure steel cylinder (1) to 60°C, the heating temperature range of the main heating zone is 25-80°C, the heating temperature range of the auxiliary heating zone is 80-120°C, the annular heating pipe (6) is wound with a spiral electromagnetic coil (61), the annular heating pipe (6) is a metal pipe.

2. A method for adding raw material liquid in a standard gas configuration, characterized in that: The raw material liquid is added using the standard gas configuration device as described in claim 1, and the addition steps are as follows: S1: Close the pressure reducing valve (11) and the valve (71) on the cylinder connector of the sample cylinder (7), open the three valves on the first three-way valve (3), open the manual valves (51) at both ends of the horizontal pipe on the second three-way valve (5) and close the manual valve (51) on the vertical pipe. S2: Heat the temperature inside the high-pressure steel cylinder (1) to 50-60℃ and the main heating zone to 70-80℃ until the temperature stabilizes; S3: Turn on the vacuum switch (41) and turn on the vacuum pump (4) to draw a vacuum. After drawing for a period of time, turn off the vacuum switch (41) in time, open the pressure reducing valve (11), and exhaust the gas into the pipeline through the high-pressure steel cylinder (1) so that the pressure of the high-purity gas in the pipeline is 0.5MPa. S4: Repeat step S3 at least 10 times to completely fill the pipeline with high-purity gas. At this time, the vacuum switch (41) is closed. S5: Close the manual valves (51) at both ends of the horizontal pipe of the second three-way valve (5), then open the manual valve (51) on the vertical pipe, inject a quantitative amount of raw material liquid into the second three-way valve (5) through the injection port of the vertical pipe using a quantitative syringe, then close the manual valve (51) on the vertical pipe, heat the second three-way valve (5) to 120°C in the auxiliary heating zone, then open the manual valves (51) at both ends of the horizontal pipe of the second three-way valve (5), and close the flow meter (2); S6: Adjust the pressure reducing valve (11) to a secondary pressure of 0.6 MPa, open the valve (71) on the cylinder connector of the sample cylinder (7), and open the flow meter (2) to adjust the flow rate to 0.5 liters / minute; S7: When the pressure of the sample cylinder (7) reaches the secondary pressure of 0.6MPa, the flow of the flow meter (2) tends to 0. Close the valve (71) on the sample cylinder (7), close the flow meter (2), close the pressure reducing valve (11), disassemble the pipeline, and complete the addition.

3. The method for adding raw material liquid in a standard gas configuration according to claim 2, characterized in that: The annular heating pipe (6) is heated by an electromagnetic coil (61). If the annular heating pipe (6) needs to be heated to a temperature higher than that of the main heating zone, it needs to be heated by the electromagnetic coil (61) and kept at the heating temperature for 10 minutes.

4. The method for adding raw material liquid in a standard gas configuration according to claim 3, characterized in that: When adding a quantitative amount of raw material liquid into the second three-way valve (5) in step S5, wear heat-resistant gloves.

5. The method for adding raw material liquid in a standard gas configuration according to claim 4, characterized in that: The heating temperatures of the main heating zone, the secondary heating zone, and the annular heating pipe (6) are adjusted according to the vaporization temperature of the added liquid and the injection volume.

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