Multi-channel solution deoxygenization device for laboratory and deoxygenization method of multi-channel solution deoxygenization device

By combining vacuum deoxygenation method and nitrogen or inert gas replacement method, the problem of time-consuming inert gas replacement method is solved, and rapid and efficient solution deoxygenation is achieved, which significantly saves resources and time.

CN119548857APending Publication Date: 2025-03-04INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202311131790.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-09-04
Publication Date
2025-03-04

AI Technical Summary

Technical Problem

The existing inert gas replacement method takes a long time to deoxygenate the solution, resulting in serious waste of laboratory resources.

Method used

The vacuum deoxygenation method is used to combine nitrogen or inert gas displacement method, and the air in the airtight container is extracted through a vacuum pump, and the nitrogen or inert gas is used for circulating replacement treatment to achieve rapid deoxygenation.

Benefits of technology

It significantly improves the deoxygenation efficiency of the solution, saves more than 90% of the gas source consumption and time, and is suitable for the laboratory's rapid deoxygenation needs.

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Abstract

The invention relates to the technical field of vacuum deoxygenization, in particular to a multichannel solution deoxygenization device for a laboratory and a deoxygenization method of the multichannel solution deoxygenization device. A pressure reducing valve, a gas source switch, a vacuum pump switch, a drying pipe, a vacuum pump and a gas cylinder are sequentially arranged on the first pipeline, one end of the first pipeline is communicated with the vacuum pump, and the other end of the first pipeline is communicated with the gas cylinder filled with nitrogen or inert gas; the first vacuum pressure gauge, the guide pipes and the second vacuum pressure gauge are sequentially arranged on the second pipeline, the eight guide pipes are installed on the second pipeline through the pipe joints respectively, the fixing platform is connected with the second pipeline through the fixing platform support, a solution sample to be deoxidized is contained in the anaerobic bottle, and the anaerobic bottle is placed on the fixing platform. And each conduit is connected with an anaerobic bottle through a needle head to remove oxygen in the solution. The method solves the problem of long time consumption of deoxidizing by an inert gas replacement method, improves the deoxidizing efficiency of the solution, saves 90% of gas source consumption, and is suitable for rapidly deoxidizing the solution in a laboratory.
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Description

Technical Field

[0001] The invention relates to the technical field of vacuum deoxygenation, in particular to a multi-channel solution deoxygenation device for a laboratory and a deoxygenation method thereof. Background Art

[0002] In order to simulate the on-site anaerobic environment, the experimental solution is generally required to be deoxygenated before the corrosion test to ensure the accuracy of the experimental data. For example: dynamic corrosion coupon weight loss test can be used to evaluate the corrosion resistance of materials, corrosion inhibitor screening and coating effects. In actual test experiments, the deoxygenation time and flow rate are uncertain, and the details of the deoxygenation process vary from person to person and are difficult to quantify, resulting in large differences in corrosion test results and poor reproducibility. The residual dissolved oxygen in the solution has an important influence on the corrosion evaluation results: on the one hand, the corrosion rate of oxygen is more than dozens of times that of CO2 and H2S gases. If the solution contains residual O2, it will have a great impact on the test results and cannot accurately evaluate the corrosion situation. On the other hand, most of the existing corrosion inhibitors do not work on oxygen corrosion, which is inconsistent with the actual application conditions, and will lead to inaccurate screening test results of corrosion inhibitors.

[0003] At present, the general corrosion testing unit laboratories in China generally adopt the inert gas replacement deoxygenation method, that is, the solution is blown with inert gas for a long time, and the solution is replaced and deoxygenated at a large flow rate for a long time, which leads to serious waste of resources and takes a long time. Summary of the invention

[0004] In view of the problems existing in the above-mentioned prior art, the purpose of the present invention is to provide a multi-channel solution deoxygenation device and a deoxygenation method for laboratory use, so as to solve the problem that the existing inert gas replacement method uses long-term nitrogen purge for deoxygenation when deoxygenating the solution, resulting in serious waste of laboratory resources and a long time consumption.

[0005] The technical solution of the present invention is:

[0006] A multi-channel solution deoxygenation device for laboratory use, the device comprises a first pipeline and a second pipeline, and the specific structure is as follows:

[0007] The first pipeline is provided with: a pressure reducing valve, a gas source switch, a vacuum pump switch, a drying tube, a vacuum pump, and a gas cylinder in sequence; one end of the first pipeline is connected to the vacuum pump, and the other end of the first pipeline is connected to a gas cylinder filled with nitrogen or an inert gas;

[0008] A first vacuum pressure gauge, a catheter, and a second vacuum pressure gauge are sequentially arranged on the second pipeline. The first vacuum pressure gauge is located at one end of the second pipeline, and the second vacuum pressure gauge is located at the other end of the second pipeline. Eight catheters are respectively installed on the second pipeline through pipe joints. The fixed platform is connected to the second pipeline through a fixed platform bracket. The sample of the solution to be deoxygenated is placed in an anaerobic bottle, and the anaerobic bottle is placed on the fixed platform. Each catheter is connected to the anaerobic bottle through a needle to deoxygenate the solution.

[0009] The laboratory multi-channel solution deoxygenation device has a three-way pipe joint in the middle of the second pipeline connected to the four-way pipe joint on the first pipeline through a pipeline, so that the second pipeline is connected to the first pipeline, the four-way pipe joint is respectively connected to the gas source switch and the second pipeline through pipelines, the four-way pipe joint is connected to the pressure reducing valve through the deoxygenating gas pipeline, and the four-way pipe joint is connected to the vacuum pump switch through the vacuum pipeline. The vacuum pipeline and the deoxygenating gas pipeline are arranged in series, and the dissolved oxygen in the anaerobic bottle solution is replaced by the vacuum pump with nitrogen or inert gas.

[0010] In the laboratory multi-channel solution deoxygenation device, the drying tube is located on the vacuum pipeline of the upper section of the vacuum pump.

[0011] The multi-channel solution deoxygenation device for laboratory use has a needle inserted into the headspace of the anaerobic bottle, and a headspace volume of not less than 10 ml is reserved above the solution to be treated in the anaerobic bottle.

[0012] A multi-channel solution deoxygenation method for laboratory use, comprising the following steps:

[0013] (1) The solution to be treated is placed in an anaerobic bottle and placed on a fixed platform before deoxygenation;

[0014] (2) The needle is inserted into the headspace of the anaerobic bottle. A single cycle includes: vacuuming the anaerobic bottle for 1 minute and replacing it with nitrogen or inert gas for 1 minute;

[0015] (3) Repeat step (2) 3 to 5 times to complete deoxygenation.

[0016] In the laboratory multi-channel solution deoxygenation method, in step (2), the gas source switch is turned off, the vacuum pump switch and the vacuum pump are turned on, and the gas in the solution to be treated is extracted for 1 minute, the vacuum pump switch is turned off, the gas source switch is turned on, and the nitrogen purge is continued for 1 minute. At this time, the first deoxygenation is completed, and the above cycle is performed 3 to 5 times.

[0017] In the laboratory multi-channel solution deoxygenation method, the vacuum pipeline and the deoxygenation gas pipeline are arranged in series and work in coordination; they cannot work simultaneously during deoxygenation.

[0018] The laboratory multi-channel solution deoxygenation method uses a dissolved oxygen probe to test the oxygen content in the solution after deoxygenation is completed.

[0019] The laboratory multi-channel solution deoxygenation method, the vacuum pump type is an oil-free silent vacuum pumping equipment, the power is 320W, the current is 2.55A, the voltage is 220V, the vacuum efficiency is 0~-0.8bar, the nitrogen deoxygenation pressure is 0.05~0.1MPa, and the flow rate is 2.5~4ml / min.

[0020] The technical principle of the present invention is:

[0021] The present invention contains a solution sample in an anaerobic bottle to maintain a certain headspace volume (at least about 10 ml), inserts a needle of each channel into the headspace of the anaerobic bottle, adopts a vacuum deoxygenation method, i.e., uses a vacuum pump to extract air from a closed container to reduce dissolved gas in water, and uses nitrogen or inert gas purging and replacement to improve deoxygenation efficiency, performs vacuum extraction and nitrogen or inert gas circulation treatment in the anaerobic bottle for 1 minute each, and repeats 3 to 5 times to complete deoxygenation.

[0022] The advantages and beneficial effects of the present invention are:

[0023] 1. The present invention is provided with two pipeline channels working in parallel, the first pipeline channel comprises a nitrogen or inert gas source and a vacuum pump, and the second pipeline comprises eight parallel working channels, and the anaerobic bottle is connected to the needle through a catheter to deoxygenate the solution.

[0024] 2. The present invention proposes a method of deoxygenating the solution by combining the vacuum method with the inert gas replacement method, which is conducive to better control of deoxygenation parameters and time, achieving the purpose of rapid deoxygenation, significantly improving the deoxygenation efficiency of the solution, and saving 90% of gas source consumption.

[0025] 3. The present invention proposes to use a drying tube to filter the water vapor and impurities in the pipeline to prevent the vacuum pump from being damaged by inhaling water vapor. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 The present invention is a schematic diagram of the structure of a multi-channel solution deoxygenation device for a laboratory. In the figure, 1, a pressure reducing valve; 2, a first pipeline (21 deoxygenation gas pipeline, 22 vacuum pipeline); 3, a gas source switch; 4, a vacuum pump switch; 5, a drying tube; 6, a vacuum pump; 7, a first vacuum pressure gauge; 8, a fixed platform bracket; 9, a catheter; 10, a needle; 11, a second pipeline; 12, a second vacuum pressure gauge; 13, a gas cylinder; 14, a fixed platform; 15, a three-way pipe joint; 16, a four-way pipe joint.

[0027] Figure 2 It is a physical picture of the multi-channel solution deoxygenation device for laboratory use of the present invention.

[0028] Figure 3 This is an efficiency comparison chart. DETAILED DESCRIPTION

[0029] like Figure 1-Figure 2 As shown, the present invention proposes a multi-channel solution deoxygenation device for laboratory use, which mainly includes: a pressure reducing valve 1, a first pipeline 2, a gas source switch 3, a vacuum pump switch 4, a drying tube 5, a vacuum pump 6, a first vacuum pressure gauge 7, a fixed platform bracket 8, a catheter 9, a needle 10, a second pipeline 11, a second vacuum pressure gauge 12, a gas cylinder 13, a fixed platform 14, etc. The specific structure is as follows:

[0030] The first pipeline 2 is provided with: a pressure reducing valve 1, a gas source switch 3, a vacuum pump switch 4, a drying tube 5, a vacuum pump 6, and a gas cylinder 13 in sequence; one end of the first pipeline 2 is connected to the vacuum pump 6, and the other end of the first pipeline 2 is connected to the gas cylinder 13 filled with nitrogen or inert gas;

[0031] A first vacuum pressure gauge 7, a conduit 9, and a second vacuum pressure gauge 12 are sequentially arranged on the second pipeline 11. The first vacuum pressure gauge 7 is located at one end of the second pipeline 11, and the second vacuum pressure gauge 12 is located at the other end of the second pipeline 11. Eight conduits 9 are respectively installed on the second pipeline 11 through pipe joints. The fixed platform 14 is connected to the second pipeline 11 through the fixed platform bracket 8. The sample of the solution to be deoxygenated is placed in an anaerobic bottle, and the anaerobic bottle is placed on the fixed platform 14. Each conduit 9 is connected to the anaerobic bottle through a needle 10 to deoxygenate the solution, and the needle 10 should be inserted into the head space of the anaerobic bottle.

[0032] The three-way pipe joint 15 in the middle of the second pipeline 11 is connected to the four-way pipe joint 16 on the first pipeline 2 through a pipeline, so that the second pipeline 11 is connected to the first pipeline 2, the four-way pipe joint 16 is respectively connected to the gas source switch 3 and the second pipeline 11 through pipelines, the four-way pipe joint 16 is connected to the pressure reducing valve 1 through the deoxygenating gas pipeline 21, and the four-way pipe joint 16 is connected to the vacuum pump switch 4 through the vacuum pipeline 22. The vacuum pipeline 22 and the deoxygenating gas pipeline 21 are arranged in series, and the dissolved oxygen in the anaerobic bottle solution is replaced by nitrogen or inert gas through the vacuum pump 6.

[0033] In the vacuum pipeline 22: the drying tube 5 is located on the vacuum pipeline 22 at the upper section of the vacuum pump 6, in order to prevent water vapor and impurities in the solution to be treated from being sucked into the vacuum pump 6 and causing malfunctions. The drying tube 5 is arranged on the vacuum pipeline 22 to effectively absorb water molecules carried in the pipeline and filter out impurities.

[0034] A certain headspace volume (not less than 10 ml) should be reserved for the solution to be treated in the anaerobic bottle, and the needle 10 should be inserted into the headspace environment of the anaerobic bottle without contacting the surface of the solution to be treated.

[0035] like Figure 1-Figure 2 As shown, the deoxygenation method of the laboratory multi-channel solution deoxygenation device of the present invention is as follows:

[0036] 1. The solution to be treated is placed in an anaerobic bottle and placed on a fixed platform 14 before deoxygenation;

[0037] 2. Needle 10 should be inserted into the headspace of the anaerobic bottle;

[0038] 3. Turn off the gas source switch 3, turn on the vacuum pump switch 4 and the vacuum pump 6, extract the gas in the solution to be treated for 1 minute, turn off the vacuum pump switch 4, turn on the gas source switch 3, and continue the nitrogen purge for 1 minute. At this time, the first deoxygenation is completed. The above cycle can be repeated 3 to 5 times to complete the deoxygenation.

[0039] 4. During deoxygenation, the power of the vacuum pump 6 is 320W, the current is 2.55A, the voltage is 220V, the vacuum degree is -0.1bar, the nitrogen deoxygenation pressure is 0.05-0.1MPa, and the flow rate is 2.5-4ml / min.

[0040] like Figure 3 As shown, the dissolved oxygen content of 1L of the solution to be treated before deoxygenation is about 8mg / L, and the dissolved oxygen content measured after 4 deoxygenation cycles by the device of the present invention is less than 1μg / L. Compared with the traditional inert gas replacement method, it takes 2 hours to deoxygenate 1L of solution, while the deoxygenation time of the device of the present invention is 8 minutes, saving more than 90% of time and inert gas consumption.

[0041] The implementation results show that the device of the present invention adopts a structure of vacuum pumping and parallel deoxygenation gas circulation, which can quickly remove dissolved oxygen in the solution, significantly improve the deoxygenation efficiency of the solution, greatly save deoxygenation time and cost, and is suitable for rapid deoxygenation of solutions in laboratories.

Claims

1. A multi-channel solution deoxygenation device for laboratory use, characterized in that: The device includes a first pipeline and a second pipeline, and the specific structure is as follows: The first pipeline is provided with: a pressure reducing valve, a gas source switch, a vacuum pump switch, a drying tube, a vacuum pump, and a gas cylinder in sequence; one end of the first pipeline is connected to the vacuum pump, and the other end of the first pipeline is connected to a gas cylinder filled with nitrogen or an inert gas; A first vacuum pressure gauge, a catheter, and a second vacuum pressure gauge are sequentially arranged on the second pipeline. The first vacuum pressure gauge is located at one end of the second pipeline, and the second vacuum pressure gauge is located at the other end of the second pipeline. Eight catheters are respectively installed on the second pipeline through pipe joints. The fixed platform is connected to the second pipeline through a fixed platform bracket. The sample of the solution to be deoxygenated is placed in an anaerobic bottle, and the anaerobic bottle is placed on the fixed platform. Each catheter is connected to the anaerobic bottle through a needle to deoxygenate the solution.

2. The multi-channel solution deoxygenation device for laboratory use according to claim 1, characterized in that: The three-way pipe joint in the middle of the second pipeline is connected to the four-way pipe joint on the first pipeline through a pipeline, so that the second pipeline is connected to the first pipeline, the four-way pipe joint is respectively connected to the gas source switch and the second pipeline through pipelines, the four-way pipe joint is connected to the pressure reducing valve through the deoxygenating gas pipeline, and the four-way pipe joint is connected to the vacuum pump switch through the vacuum pipeline. The vacuum pipeline and the deoxygenating gas pipeline are arranged in series, and the dissolved oxygen in the anaerobic bottle solution is extracted by replacing with nitrogen or inert gas through the vacuum pump.

3. The multi-channel solution deoxygenation device for laboratory use according to claim 1, characterized in that: The drying tube is located on the vacuum pipeline at the upper section of the vacuum pump.

4. The multi-channel solution deoxygenation device for laboratory use according to claim 1, characterized in that: The needle is inserted into the headspace of the anaerobic bottle, and a headspace volume of not less than 10 ml is reserved above the solution to be treated in the anaerobic bottle.

5. A laboratory multi-channel solution deoxygenation method using the device according to any one of claims 1 to 4, characterized in that: The steps include: (1) The solution to be treated is placed in an anaerobic bottle and placed on a fixed platform before deoxygenation; (2) The needle is inserted into the headspace of the anaerobic bottle. A single cycle includes: vacuuming the anaerobic bottle for 1 minute and replacing it with nitrogen or inert gas for 1 minute; (3) Repeat step (2) 3 to 5 times to complete deoxygenation.

6. The method for deoxygenating a multi-channel solution for laboratory use according to claim 5, characterized in that: In step (2), turn off the gas source switch, turn on the vacuum pump switch and the vacuum pump, extract the gas in the solution to be treated for 1 minute, turn off the vacuum pump switch, turn on the gas source switch, and continue nitrogen purging for 1 minute. At this time, the first deoxygenation is completed, and the above cycle is performed 3 to 5 times.

7. The method for deoxygenating a multi-channel solution for laboratory use according to claim 5, characterized in that: The vacuum pipeline and the deoxygenating gas pipeline are arranged in series and work together; they cannot work at the same time during deoxygenation.

8. The method for deoxygenating a multi-channel solution for laboratory use according to claim 5, characterized in that: After deoxygenation is complete, a dissolved oxygen probe is used to test the oxygen content in the solution.

9. The method for deoxygenating a multi-channel solution for a laboratory according to claim 5, characterized in that: The vacuum pump is an oil-free silent vacuum pumping device with a power of 320W, a current of 2.55A, a voltage of 220V, a vacuum efficiency of 0 to -0.8bar, a nitrogen deoxygenation pressure of 0.05 to 0.1MPa, and a flow rate of 2.5 to 4ml / min.

Citation Information

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