A carbon monoxide purification system and purification method

Abstract

The application discloses a carbon monoxide purification system and a purification method, and relates to the technical field of carbon monoxide preparation. The carbon monoxide purification system comprises a gas source, a low-temperature cold trap and a purification device. The gas source is overhead gas of an isotopic primary rectifying column; the low-temperature cold trap is communicated with the gas source and is used for removing part of impurities in the overhead gas; and the purification device is communicated with an output end of the low-temperature cold trap and is used for reducing metal ions in the overhead gas. The carbon monoxide purification system provided by the application can effectively remove gas-phase impurities and metal ions in carbon monoxide gas by adopting the combination of the low-temperature cold trap and the purifier, thereby not only avoiding the investment cost of using low-temperature rectifying equipment, but also reducing the liquid nitrogen energy consumption caused by using the low-temperature rectifying equipment, and the whole process is simpler and more efficient.

Description

Technical Field

[0001] This application relates to the field of carbon monoxide preparation technology, and in particular to a carbon monoxide purification system and purification method. Background Technology

[0002] Electronic-grade carbon monoxide is a key raw material widely used in high-tech fields such as semiconductors, photovoltaics, and fine chemicals. The content of impurities in it is subject to extremely strict requirements, especially metal ion impurities, as their residues can seriously affect the performance and reliability of the final product.

[0003] To achieve efficient purification of carbon monoxide, cryogenic distillation is widely used in industry. Cryogenic distillation involves operating at low temperatures near the boiling point of carbon monoxide. Carbon monoxide gas containing impurities is introduced into a distillation column, and the components are separated step-by-step based on their boiling point differences, thus obtaining a high-purity carbon monoxide product. However, this method is costly in removing metal ions from the electronic-grade carbon monoxide feed gas. Summary of the Invention

[0004] In view of this, this application provides a carbon monoxide purification system and a carbon monoxide purification method, with the aim of solving one of the technical problems in the prior art.

[0005] To achieve the above objectives, the technical solution adopted in this application is as follows:

[0006] In a first aspect, this application provides a carbon monoxide purification system, comprising:

[0007] The gas source is the overhead gas from a primary isotope distillation column;

[0008] A low-temperature cold trap is connected to the gas source and is used to remove some impurities from the gas at the top of the tower.

[0009] A purification device is connected to the output end of the cryogenic cold trap, and the purification device is used to reduce the metal ions in the overhead gas of the tower.

[0010] In an optional embodiment, the carbon monoxide purification system further includes:

[0011] A vacuum pumping device is connected to the input and output ends of the purification device. The vacuum pumping device is used to evacuate the pipelines of the purification device, the front end of the purification device, and the rear end of the purification device.

[0012] In an optional embodiment, the carbon monoxide purification system further includes:

[0013] A purging device is connected to the input end of the purification device, and the purging device is used to purge gas from the purification device.

[0014] An analytical device is provided at the output end of the purification device, and the analytical device is used to analyze the gas components output by the purification device.

[0015] In an optional embodiment, the carbon monoxide purification system further includes:

[0016] The first filter is located at the input end of the cryogenic cold trap and is connected to the gas source;

[0017] The second filter is connected to the output end of the cryogenic cold trap.

[0018] In an optional embodiment, the vacuum device includes a first venting pipe, a second venting pipe, and a third venting pipe. The first venting pipe is connected to the input end of the purification device, the second venting pipe is connected to the output end of the first filter, and the third venting pipe is connected to the output end of the purification device.

[0019] In an optional embodiment, the carbon monoxide purification system further includes:

[0020] A buffer, wherein the buffer is connected to the output of the second filter;

[0021] The compressor has its input end connected to the output end of the buffer, and its output end is connected to the input end of the purification device.

[0022] In an optional embodiment, the carbon monoxide purification system further includes:

[0023] The first pressure transmitter is located at the input end of the first filter;

[0024] A second pressure transmitter is located at the output end of the buffer.

[0025] A first mass flow meter is installed at the input end of the cryogenic cold trap;

[0026] A second mass flow meter is located at the input end of the purification device.

[0027] In an optional embodiment, the carbon monoxide purification system further includes a gas collection container and an emergency shut-off valve, wherein the emergency shut-off valve is connected to the output end of the purification device, and the gas collection container is connected to the output end of the emergency shut-off valve.

[0028] Secondly, this application provides a carbon monoxide purification method using any of the carbon monoxide purification systems described in the foregoing embodiments, comprising:

[0029] The gas source was the top gas of the isotope primary tower.

[0030] Vacuum the purification device and its front and rear pipelines separately.

[0031] The purification device is purged with a standard-compliant test gas. The purging is continued until the analysis results of the purge gas components by the analytical device meet the standard.

[0032] Start the cryogenic cold trap;

[0033] The top gas of the isotope primary column is injected, and the top gas passes sequentially through a cryogenic cold trap and a purification device.

[0034] In optional implementations, at least one of the following is also included:

[0035] The operating temperature of the cryogenic cold trap is -15℃ to -10℃;

[0036] The gas flow rate input to the purification unit is 0.5-0.75 kg / h;

[0037] The purification device includes multiple sets of purifiers, each set of purifiers is started sequentially, the purging time of each set of purifiers should be no less than 1 hour, the purging flow rate is 0.5~2 kg / h, and the purging pressure is no less than 0.5 MPa;

[0038] After replacing the purifier, the initial purging time should be no less than 10 hours, the purging flow rate should be 0.5~2 kg / h, and the purging pressure should be no less than 0.5 MPa.

[0039] Compared to existing technologies, the advantages of this application are as follows: This application proposes a carbon monoxide purification system, including a gas source, a cryogenic cold trap, and a purification device. The gas source is the overhead gas from an isotope primary distillation column; the cryogenic cold trap is connected to the gas source and is used to remove some impurities from the overhead gas; the purification device is connected to the output of the cryogenic cold trap and is used to reduce metal ions in the overhead gas. By first "freezing" impurities such as moisture, oxygen, and nitrogen from the overhead gas through the cryogenic cold trap, some impurities are removed. Then, the resin material (such as a strongly acidic cation exchange resin or an ammonium phosphate chelating resin) within the purification component efficiently adsorbs and removes metal ions (such as iron and nickel). The combination of the cryogenic cold trap and the purifier effectively removes gaseous impurities and metal ions from carbon monoxide gas, avoiding the investment costs of cryogenic distillation equipment and reducing the liquid nitrogen energy consumption associated with such equipment. The entire process is simpler and more efficient. Attached Figure Description

[0040] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0041] Figure 1 The following are schematic diagrams of the carbon monoxide purification system in some embodiments of this application;

[0042] Figure 2 A flowchart of a carbon monoxide purification method in some embodiments of this application is shown.

[0043] Key component symbols: 100 - Carbon monoxide purification system; 110 - Gas source; 120 - Cryogenic cold trap; 130 - Purification device; 141 - Vacuum assembly; 150 - Purge device; 160 - Analytical device; 171 - First filter; 1411 - First vent line; 1412 - Second vent line; 1413 - Third vent line; 180 - Buffer; 190 - Compressor; A1 - First safety valve; A2 - Second safety valve; B1 - First pressure transmitter; B2 - Second pressure transmitter; C1 - First mass flow meter; C2 - Second mass flow meter; 131 - Purifier; E - Gas collection container; D1 - Emergency shut-off valve; V1 - First valve; V2 - Second valve; V3 - Third valve; V4 - Fourth valve; V5 - Fifth valve; V6 - Sixth valve; V7 - Seventh valve; V8 - Eighth valve; V9 - Ninth valve; V10 - Tenth valve; V11 - Eleventh valve; V12 - Twelfth valve; V13 - Thirteenth valve; V14 - Fourteenth valve; V15 - Fifteenth valve; V16 - Sixteenth valve; V17 - Seventeenth valve; V18 - Eighteenth valve; V19 - Nineteenth valve; V20 - Twentieth valve; V21 - Twenty-first valve; V22 - Twenty-second valve; V23 - Twenty-third valve; V24 - Twenty-fourth valve; 172 - Second filter; V0 - Initial valve; 142 - Vacuum pump; F - Evacuation device. Detailed Implementation

[0044] The embodiments of this application are described in detail below. Examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain this application, and should not be construed as limiting this application.

[0045] In the description of this application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., indicating the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the system or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this application.

[0046] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this application, "multiple" means two or more, unless otherwise explicitly specified.

[0047] In this application, unless otherwise expressly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.

[0048] In this application, unless otherwise expressly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "on top of," and "over" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.

[0049] In the isotope primary tower 13 CO isotopes, 12 The low separation coefficient between CO isotopes, the narrow column diameter, the high column height, and the long gas exchange and residence time make it easy for carbon monoxide (CO) to react with the metal surfaces inside the column, generating trace amounts of gaseous carbonyl iron, carbonyl nickel, and other metal ion impurities. This adversely affects the gas purity, making it difficult to meet the high purity requirements of electronic-grade carbon monoxide.

[0050] In related technologies, distillation columns are typically used to separate and purify impurities in carbon monoxide to remove gaseous impurities and metal ion contamination. This method requires liquid nitrogen as a refrigerant to achieve cryogenic operation, resulting in high energy consumption and long preparation times for system start-up and shutdown, thus increasing overall production costs.

[0051] In response to the above problems, such as Figure 1 As shown, an embodiment of this application provides a carbon monoxide purification system 100, which mainly utilizes the overhead gas from an isotope primary distillation column to produce electronic-grade carbon monoxide that meets standards. The carbon monoxide purification system 100 includes a gas source 110, a cryogenic cold trap 120, and a purification device 130.

[0052] Among them, gas source 110 is the overhead gas from the isotope primary distillation column. During the isotope separation process... 13 CO is mainly concentrated at the bottom of the tower, while the isotopic primary gas is concentrated at the top of the tower. 13 The CO abundance is low, so the overhead gas from the first-stage column cannot be recovered for use. 13 The purification of CO isotopes requires complete recovery into the tail gas system, where they are mixed with other tail gases and ultimately sold as ordinary carbon monoxide. This application transforms the overhead gas from the isotope primary distillation column, which was originally considered waste, into a high-value electronic-grade gas, thereby improving economic efficiency.

[0053] The low-temperature cold trap 120 is connected to the gas source 110 and is used to remove some impurities from the overhead gas. The purification device 130 is connected to the output end of the low-temperature cold trap 120 and is used to reduce metal ions in the overhead gas.

[0054] This application first uses a cryogenic cold trap 120 to freeze impurities such as moisture, oxygen, and nitrogen from the top gas of an isotope primary distillation column, removing some of the impurities. Then, a purification unit is used to efficiently remove metal ions (such as iron and nickel). The combination of the cryogenic cold trap 120 and the purifier 131 effectively removes gaseous impurities and metal ions from carbon monoxide gas, resulting in carbon monoxide gas with impurity content conforming to the national standard GB / T43771-2024 "Electronic Gases - Carbon Monoxide". This not only avoids the investment costs of using cryogenic distillation equipment but also reduces the liquid nitrogen energy consumption associated with such equipment, making the entire process simpler and more efficient.

[0055] In some embodiments, the carbon monoxide purification system 100 further includes a vacuum device. The vacuum device includes a vacuum assembly 141 and a vacuum pump 142.

[0056] like Figure 1As shown, the vacuum assembly 141 is connected to the input and output terminals of the purification device 130. The vacuum assembly 141 is also connected to the vacuum pump 142, and performs vacuuming on the purification device 130, the pipelines at the front and rear ends of the purification device 130. This reduces the impact of residual gas in the system on the purification effect and improves the stability and purity output of the purification device 130.

[0057] The front end of the purification device 130 refers to the gas input end of the purification device 130, and the rear end of the purification device 130 refers to the gas output end of the purification device 130.

[0058] In some embodiments, the carbon monoxide purification system 100 further includes a purging device 150 and an analysis device 160.

[0059] like Figure 1 As shown, the purging device 150 is connected to the input end of the purification device 130. The purging device 150 is used to purge the purification device 130 with gas to remove residues or impurities from the pipeline. The analysis device 160 is located at the output end of the purification device 130. The analysis device 160 is used to analyze the gas components output by the purification device 130 to determine whether the purging is complete. For example, the analysis device 160 is also used to perform real-time analysis of the purge gas components output by the purification device 130 to determine whether the purging is complete; or, for example, the analysis device 160 is used to perform real-time analysis of the components of the overhead gas output by the purification device 130 to improve the stability of the product output of the carbon monoxide purification system 100.

[0060] In some embodiments, the gas purged by the purging device 150 is finished electronic-grade carbon monoxide gas.

[0061] In some embodiments, the carbon monoxide purification system 100 further includes a first filter 171 and a second filter 172.

[0062] like Figure 1 As shown, the first filter 171 is located at the input end of the cryogenic cold trap 120 and is connected to the gas source 110; the second filter 172 is connected to the output end of the cryogenic cold trap 120. The first filter 171 performs preliminary filtration of carbon monoxide output from the isotope primary column, removing particulate matter and other impurities. The cryogenic cold trap 120 further removes volatile impurities from the gas through cryogenic cooling. The second filter 172 performs secondary filtration of the carbon monoxide after treatment by the cryogenic cold trap 120, improving the purity of the gas.

[0063] In this embodiment, both the first filter 171 and the second filter 172 are filters using PTFE (polytetrafluoroethylene) material as the filler, and the filtration accuracy can reach 0.03μm.

[0064] In other embodiments, the first filter 171 and the second filter 172 may also be HEPA (High Efficiency Particulate Air) filters, molecular sieve filters, membrane filters, nanofiber filters, etc.

[0065] like Figure 1 As shown, an initial valve V0 and a first valve V1 are sequentially installed between the top gas output pipeline of the isotope primary tower and the first filter 171 to control the opening and closing of the pipeline. A third valve V3 is installed between the first filter 171 and the cryogenic cold trap 120 to control the opening and closing of the pipeline. A fourth valve V4 is installed between the cryogenic cold trap 120 and the second filter 172 to control the opening and closing of the pipeline.

[0066] In some embodiments, the vacuum assembly 141 includes a first venting conduit 1411, a second venting conduit 1412, and a third venting conduit 1413.

[0067] like Figure 1 As shown, the input end of the first venting pipeline 1411 is connected to the input end of the purification device 130, and the output end is connected to the interface of the vacuum pump 142; the input end of the second venting pipeline 1412 is connected to the output end of the first filter 171, and the output end is connected to the first venting pipeline 1411; the input end of the third venting pipeline 1413 is connected to the output end of the purification device 130, and the output end is connected to the second venting pipeline 1412.

[0068] In one embodiment, such as Figure 1 As shown, the second venting pipe 1412, the cryogenic cold trap 120, the second filter 172 and the first venting pipe 1411 are connected in sequence. The vacuum pump 142 performs a vacuum operation on the front end pipe of the purification device 130 to remove N2, O2, Ar, H2O, CO2 and other possible particulate matter in the pipe, reduce the impact of residual gas in the system on the purification effect, and improve the stability and purity output of the purification device 130.

[0069] In one embodiment, such as Figure 1 As shown, the third exhaust pipe 1413 is connected to the second exhaust pipe 1412. The first exhaust pipe 1411, the purification device 130, the third exhaust pipe 1413, and the second exhaust pipe 1412 are connected in sequence. The vacuum pump 142 performs a vacuum operation on the purification device 130 and the pipeline at the rear end of the purification device 130 to remove N2, O2, Ar, H2O, CO2, and other possible particulate matter from the pipeline, thereby reducing the impact of residual gas in the system on the purification effect and improving the stability and purity output of the purification device 130.

[0070] See Figure 1The first vent pipe 1411 is equipped with an eighth valve V8 to control the opening and closing of the pipe, the second vent pipe 1412 is equipped with a second valve V2 to control the opening and closing of the pipe, and the third vent pipe 1413 is equipped with a twenty-second valve V22 to control the opening and closing of the pipe.

[0071] In some embodiments, the carbon monoxide purification system 100 further includes a buffer 180 and a compressor 190.

[0072] like Figure 1 As shown, the buffer 180 is connected to the output end of the second filter 172. The buffer 180 smooths the pressure fluctuations generated during the operation of the compressor 190 by storing and releasing gas, so that the gas pressure received by the compressor 190 is more uniform.

[0073] In one embodiment, such as Figure 1 As shown, a fifth valve V5 controls the on / off state of the pipeline between the second filter 172 and the buffer 180. The buffer 180 has two discharge pipelines, one of which is connected to the compressor 190 and also to the first vent pipeline 1411 and the second vent pipeline 1412. A seventh valve V7 controls the on / off state of the pipeline between the buffer 180 and the second vent pipeline 1412, and a ninth valve V9 controls the on / off state of the pipeline between the buffer 180 and the compressor 190. A sixth valve V6 and a first safety valve A1 are installed on the other discharge pipeline. The sixth valve V6 controls the on / off state of the pipeline, and the first safety valve A1 is used to open when the pressure inside the buffer 180 exceeds its maximum permissible operating pressure (MAWP), allowing the gas to be directly discharged to the atmosphere or a safer location, preventing the buffer 180 from exploding.

[0074] The input end of compressor 190 is connected to the output end of buffer 180, and the output end of compressor 190 is connected to the input end of purification device 130. Compressor 190 provides a stable high-pressure gas source 110 for purification device 130.

[0075] The compressor 190 is equipped with a tenth valve V10 at its output end to control the opening and closing of the pipeline, and the tenth valve V10 is located between the compressor 190 and the input end of the first vent pipeline 1411. The purging device 150 is located between the input end of the first vent pipeline 1411 and the input end of the purification device 130.

[0076] An eleventh valve V11 is installed at the purge gas outlet of the purging device 150 to control the on / off of the pipeline.

[0077] In some embodiments, the carbon monoxide purification system 100 further includes a first pressure transmitter B1, a second pressure transmitter B2, a first mass flow meter C1, and a second mass flow meter C2.

[0078] The first pressure transmitter B1 is located at the input end of the first filter 171 and is used to measure the pressure of the gas entering the first filter 171, ensuring that the first filter 171 operates within a safe and efficient range. For example, the first pressure transmitter B1 may be an Emerson 1151, a Rosemount 3051, or a Siemens SITRANS P.

[0079] The first mass flow meter C1 is installed at the input end of the cryogenic cold trap 120 to measure the mass flow rate of carbon monoxide entering the cryogenic cold trap 120, effectively monitoring and controlling the flow rate of carbon monoxide gas entering the cold trap, thereby improving the stability and efficiency of the system. For example, the first mass flow meter C1 is a thermal mass flow meter (such as a Bronkhorst F-201CV).

[0080] The second pressure transmitter B2 is located at the output of the buffer 180 and upstream of the ninth valve V9. It is used to monitor the gas pressure input to the compressor 190, ensuring that the compressor 190 operates within a safe and efficient range. For example, the second pressure transmitter B2 may be an Emerson 1151, a Rosemount 3051, or a Siemens SITRANS P.

[0081] The second mass flow meter C2 is located at the input end of the purification device 130 and is positioned at the rear end of the purging device 150. A twelfth valve V12 is installed at the input end of the second mass flow meter C2 to control the flow of the pipeline. The second mass flow meter C2 monitors and controls the flow rate of carbon monoxide gas entering the purification device 130, improving the stability and efficiency of the system. For example, the second mass flow meter C2 is a thermal mass flow meter (such as a Bronkhorst F-201CV).

[0082] The purification device 130 includes multiple sets of purifiers 131. Each set of purifiers 131 is equipped with valves at its input and output ends to control the opening and closing of the pipeline. The multiple sets of purifiers 131 can be connected in series or in parallel as needed.

[0083] In one embodiment, such as Figure 1 As shown, the purification device 130 includes two sets of purifiers 131, with the first set of purifiers 131 and the second set of purifiers 131 connected in parallel. A thirteenth valve V13 is installed at the input end of the first set of purifiers 131, and a fourteenth valve V14 is installed at the output end of the first set of purifiers 131 to control the on / off state of the pipeline. A fifteenth valve V15 is installed at the input end of the second set of purifiers 131, and a sixteenth valve V16 is installed at the output end of the second set of purifiers 131. By setting multiple sets of valves in coordination, the switching control of multiple sets of purifiers 131 can be achieved.

[0084] In some embodiments, the carbon monoxide purification system 100 further includes a gas collection container E and an emergency shut-off valve D1, wherein the emergency shut-off valve D1 is connected to the output end of the purification device 130, and the gas collection container E is connected to the output end of the emergency shut-off valve D1.

[0085] like Figure 1 As shown, a seventeenth valve V17 is installed at the output end of the purification device 130. The output end of the seventeenth valve V17 is sequentially connected to the eighteenth valve V18, the emergency shut-off valve D1, the twenty-fourth valve V24, and the gas collection container E. This route is used to collect the purified product gas.

[0086] In this embodiment, all pipes, devices, and containers are made of 316L stainless steel with electropolished material to reduce or even prevent metal contamination with carbon monoxide gas.

[0087] The gas collection container E is made of aluminum alloy to avoid introducing metal impurities.

[0088] In some embodiments, such as Figure 1 As shown, before purifying and collecting the finished gas, the purification device 130 and the pipeline at the back end of the purification device 130 need to be purged to remove residues or impurities in the pipeline and improve the purity of the carbon monoxide purification system 100.

[0089] In one embodiment, such as Figure 1 As shown, an outlet pipe is installed between the seventeenth valve V17 and the eighteenth valve V18 to connect with the interface of the external venting device F. A nineteenth valve V19 is installed at the interface of the venting device F to discharge the exhaust gas generated during the purging process.

[0090] After purging for a period of time, the composition of the purged gas needs to be tested to determine whether the purification component has been completely purged.

[0091] In one embodiment, such as Figure 1 As shown, a parallel pipeline is connected at the outlet pipeline, and a twentieth valve V20 is installed on the parallel pipeline. The parallel pipeline is connected to the output end of the emergency shut-off valve D1. The connection point between the emergency shut-off valve D1 and the twenty-fourth valve V24 serves as the input end of the third vent pipeline 1413. An inlet for the analysis device 160 is provided on the third vent pipeline 1413, and a twenty-third valve V23 is installed at the inlet of the analysis device 160. Thus, the purged gas sequentially enters the analysis device 160 through the twentieth valve V20 and the twenty-third valve V23. The analysis device 160 analyzes whether the gas composition meets the standards for the finished product gas. In this embodiment, the purging gas for the purging device 150 is finished electronic-grade carbon monoxide that meets the standards.

[0092] A pressure relief pipeline is also connected to the parallel pipeline, and a twenty-first valve V21 and a second safety valve A2 are installed sequentially on the pressure relief pipeline. The second safety valve A2 can quickly and safely discharge gas from the pipeline in an emergency, preventing dangerous situations from occurring.

[0093] It is understood that carbon monoxide is a flammable gas. The emergency shut-off valve D1 is used to quickly and automatically cut off the flow of fluid (gas, liquid or powder) in the pipeline in the event of a dangerous situation, thereby isolating the source of danger, preventing the accident from escalating or worsening, and protecting the carbon monoxide purification system 100.

[0094] like Figure 1 and Figure 2 As shown, this application provides a carbon monoxide purification method using any of the carbon monoxide purification systems described in the foregoing embodiments, comprising:

[0095] Step S10: Use the top gas of the isotope primary column as the gas source 110.

[0096] Table 1

[0097] Unit: ppm

[0098]

[0099] Table 1 discloses the composition of the overhead gas of the isotope primary column. It is not difficult to find that the content of iron and nickel in the overhead gas does not meet the standard for electronic grade carbon monoxide, while the content of the other components does.

[0100] Step S20: Vacuum the purification device 130 and its front and rear pipelines to remove N2, O2, Ar, H2O, CO2 and other possible particulate matter from the carbon monoxide purification system 100.

[0101] Step S30: Purify the purification device 130 by purging the gas with a standard-compliant test gas (e.g., electronic-grade carbon monoxide gas). Purging continues until the analysis results of the purge gas components by the analysis device 160 meet the standard, at which point purging is stopped.

[0102] The purification device 130 and its downstream pipeline are purged with electronic-grade carbon monoxide gas. The analysis device 160 analyzes the components of the purged gas. The purging operation is completed when the analysis results meet the electronic-grade carbon monoxide standard.

[0103] The entire purification unit 130 should be purged for at least 1 hour, with a purging flow rate of 0.5~2 kg / h and a purging pressure of at least 0.5 MPa.

[0104] Step S40: Start the cryogenic cold trap 120.

[0105] In some embodiments, the operating temperature of the cryogenic cold trap 120 is -15°C to -10°C. Specifically, the operating temperature of the cryogenic cold trap 120 is -15°C, -14°C, -13°C, -12°C, -11°C, -10°C, etc., and is not limited to the examples.

[0106] In step S50, the top gas of the isotope primary column is injected, and the top gas passes sequentially through the low-temperature cold trap 120 and the purification device 130.

[0107] First, impurities such as moisture, oxygen, and nitrogen in the top gas of the isotope primary distillation column are "frozen" in a cryogenic cold trap 120, removing some of the impurities. Then, the resin material (such as a strong acid cation exchange resin or an ammonium phosphate chelating resin) in the purification component efficiently adsorbs and removes metal ions (such as iron and nickel). The combination of the cryogenic cold trap 120 and the purifier 131 effectively removes gaseous impurities and metal ions from carbon monoxide gas, and the impurity content of the produced carbon monoxide gas fully complies with the national standard GB / T43771-2024 Electronic Gas Carbon Monoxide. This not only avoids the investment costs of using cryogenic distillation equipment but also reduces the liquid nitrogen energy consumption associated with it, making the entire process simpler and more efficient.

[0108] In some embodiments, the gas flow rate input to the purification device 130 is 0.5-0.75 kg / h.

[0109] During the purification process of the top gas of the isotope primary column, only one set of purifiers 131 in the purification device 130 is started.

[0110] During the purification of the overhead gas in the isotope primary column, after replacing purifier 131, purification unit 130 should be re-purged. The purging time should be no less than 10 hours, the purging flow rate should be 0.5~2 kg / h, and the purging pressure should be no less than 0.5 MPa. At this time, the purging gas can be replaced with nitrogen to reduce costs.

[0111] The method of using the carbon monoxide purification system 100 of this application is as follows:

[0112] Before starting the system, close the initial valve V0, the sixth valve V6, the eleventh valve V11, and the twelfth valve V12. Open the valves from the first valve V1 to the fifth valve V5 and from the seventh valve V7 to the tenth valve V10 to evacuate the front end of the purification device 130. Close the seventeenth valve V17, the nineteenth valve V19, and the twenty-first valve V21. Open the eighteenth valve V18, the twentieth valve V20, the twenty-second valve V22, and the gas collection container E valve to evacuate the rear end of the purification device 130 and the gas collection container E. This removes N2, O2, Ar, H2O, CO2, and other particulate matter that may be present in the system.

[0113] After the vacuuming is completed, close the tenth valve V10, the eighteenth valve V18, and the twentieth valve V20, and open the eleventh valve V11, the twelfth valve V12, the thirteenth valve V13, the fourteenth valve V14, the fifteenth valve V15, the sixteenth valve V16, the seventeenth valve V17, the eighteenth valve V18, and the nineteenth valve V19. Open the outlet of the purging device 150 to purge the purification device 130.

[0114] After purging is complete, close the nineteenth valve V19, open the twentieth valve V20 and the twenty-third valve V23, and connect the purging gas to the analysis device 160. If the analysis shows that the gas composition is no different from that of the finished electronic-grade carbon monoxide gas, the purging is complete; otherwise, continue purging.

[0115] During the purging process, the entire purification unit 130 is purged. After purging, the valves at the input and output ends of one set of purifiers 131 are closed. Only one set of purifiers 131 is used during operation. When one set of purifiers 131 fails, another set is activated. After replacing purifier 131, the purging gas can be replaced with nitrogen to purge the entire purification unit 130. The purging process remains the same.

[0116] After vacuuming and purging, start the cryogenic cold trap 120. Once the parameters of the cryogenic cold trap 120 have stabilized, inject the top gas from the isotope primary column into the buffer 180. Keep the second valve V2, the seventh valve V7, and the ninth valve V9 closed, and open the initial valve V0, the first valve V1, the second valve V2, the third valve V3, the fourth valve V4, the fifth valve V5, and the sixth valve V6. After the second pressure transmitter B2 stabilizes, prepare to start the compressor 190. The operating temperature of the cryogenic cold trap 120 is -15℃ to -10℃. Specifically, the operating temperatures of the cryogenic cold trap 120 are -15℃, -14℃, -13℃, -12℃, -11℃, -10℃, etc., and are not limited to the examples provided.

[0117] Before starting the compressor 190, keep valves V8, V11, V19, V20, and V22 closed, and open valves V9, V10, V12, V13, V14, V17, V18, V23, V24, and the inlet valve of the gas collection container E.

[0118] The compressor 190 starts and maintains the operation of one set of purifiers 131. The valves at the input and output ends of the other set of purifiers 131 are normally closed. The input end of the purification device 130 is controlled by the second mass flow meter C2 to maintain the sample injection flow rate and mass matching the function of the purifier 131. During implementation, the flow rate is maintained at 0.5-0.75 kg / h.

[0119] Valve V23 is normally open. The gas phase impurity content can be monitored in real time through an online analysis system. It can also be connected to an external absorbent to monitor the metal ion content in the gas during the filling process.

[0120] Implementation Column 1

[0121] An inlet pressure of 0.1 MPa and an inlet flow rate of 0.5 Kg / h were used. The cryogenic cold trap 120 was maintained at -15℃. The gas was filled using an aluminum alloy cylinder. The gas detection method adopted was GB / T43771-2024 Electronic Gases Carbon Monoxide. ND means not detected (below the instrument detection limit of 0.01 ppm).

[0122] Table 2

[0123] Unit: ppm

[0124]

[0125] Table 2 discloses the electronic grade carbon monoxide gas composition standard, the gas composition of the top gas of the isotope primary column, and the gas composition of the top gas of the isotope primary column after purification by the carbon monoxide purification system of this application. It is easy to see that the contents of iron and nickel in the treated top gas are reduced, so that the contents of iron and nickel and the other components in the treated top gas meet the electronic grade carbon monoxide standard.

[0126] Implement column 2

[0127] An inlet pressure of 0.11 MPa and an inlet flow rate of 0.65 kg / h were used. The cryogenic cold trap 120 was maintained at -13°C. The gas was filled using an aluminum alloy cylinder. The gas detection method adopted was GB / T43771-2024 Electronic Gases - Carbon Monoxide. ND means not detected (below the instrument detection limit of 0.01 ppm).

[0128] Table 3

[0129] Unit: ppm

[0130]

[0131] Table 3 discloses the standard for electronic-grade carbon monoxide gas composition, the gas composition of the top gas of the isotope primary column, and the gas composition of the top gas of the isotope primary column after purification by the carbon monoxide purification system of this application. It is easy to see that the contents of iron and nickel in the treated top gas are reduced, so that the contents of iron and nickel and the other components in the treated top gas meet the standard for electronic-grade carbon monoxide.

[0132] Implement column 3

[0133] An inlet pressure of 0.09 MPa and an inlet flow rate of 0.75 Kg / h were used. The cryogenic cold trap 120 was maintained at -10℃. The gas was filled using an aluminum alloy cylinder. The gas detection method adopted was GB / T43771-2024 Electronic Gases - Carbon Monoxide. ND means not detected (below the instrument detection limit of 0.01 ppm).

[0134] Table 4

[0135] Unit: ppm

[0136]

[0137] Table 4 discloses the standard for electronic-grade carbon monoxide gas composition, the gas composition of the top gas of the isotope primary column, and the gas composition of the top gas of the isotope primary column after purification by the carbon monoxide purification system of this application. It is easy to see that the contents of iron and nickel in the treated top gas are reduced, so that the contents of iron and nickel and the other components in the treated top gas all meet the standard for electronic-grade carbon monoxide.

[0138] Referring to Examples 1 to 3, the carbon monoxide gas obtained by the carbon monoxide gas purification method of this application fully complies with "GB / T43771-2024 Electronic Gas Carbon Monoxide". Furthermore, this application avoids the investment costs of using cryogenic distillation equipment and also reduces the liquid nitrogen energy consumption caused by using cryogenic distillation equipment. The whole process is simpler and more efficient, significantly reducing costs.

[0139] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0140] Although embodiments of this application have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting this application. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of this application.

Claims

1. A carbon monoxide purification system, characterized in that, include: The gas source is the overhead gas from a primary isotope distillation column; A low-temperature cold trap is connected to the gas source and is used to remove some impurities from the gas at the top of the tower. A purification device is connected to the output end of the low-temperature cold trap, and the purification device is used to reduce metal ions in the overhead gas of the column. A vacuum pumping device is connected to the input and output ends of the purification device. The vacuum pumping device is used to evacuate the purification device, the front end of the purification device, and the rear end of the purification device. The first filter is located at the input end of the cryogenic cold trap and is connected to the gas source; A second filter is connected to the output end of the cryogenic cold trap; The vacuum device includes a first venting pipe, a second venting pipe, and a third venting pipe. The first venting pipe is connected to the input end of the purification device, the second venting pipe is connected to the output end of the first filter, and the third venting pipe is connected to the output end of the purification device.

2. The carbon monoxide purification system according to claim 1, characterized in that, The carbon monoxide purification system also includes: A purging device is connected to the input end of the purification device, and the purging device is used to purge gas from the purification device. An analytical device is provided at the output end of the purification device, and the analytical device is used to analyze the gas components output by the purification device.

3. The carbon monoxide purification system according to claim 1, characterized in that, The carbon monoxide purification system also includes: A buffer, wherein the buffer is connected to the output of the second filter; The compressor has its input end connected to the output end of the buffer, and its output end is connected to the input end of the purification device.

4. The carbon monoxide purification system according to claim 3, characterized in that, The carbon monoxide purification system also includes: The first pressure transmitter is located at the input end of the first filter; A second pressure transmitter is located at the output end of the buffer. A first mass flow meter is installed at the input end of the cryogenic cold trap; A second mass flow meter is located at the input end of the purification device.

5. The carbon monoxide purification system according to any one of claims 1 to 4, characterized in that, The carbon monoxide purification system also includes a gas collection container and an emergency shut-off valve. The emergency shut-off valve is connected to the output end of the purification device, and the gas collection container is connected to the output end of the emergency shut-off valve.

6. A method for purifying carbon monoxide using the carbon monoxide purification system according to any one of claims 2 to 5, characterized in that, include: The gas source was the top gas of the isotope primary tower. Vacuum the purification device and its front and rear pipelines separately. The purification device is purged with test gas that meets the standard. Purging is continued until the analysis results of the components of the purging gas by the analytical device meet the standard, and then purging is stopped. Start the cryogenic cold trap; The top gas of the isotope primary column is injected, and the top gas passes sequentially through a cryogenic cold trap and a purification device.

7. The carbon monoxide purification method according to claim 6, characterized in that, It also includes at least one of the following: The operating temperature of the cryogenic cold trap is -15℃ to -10℃; The gas flow rate input to the purification unit is 0.5-0.75 kg / h; The purification device includes multiple sets of purifiers, each set of purifiers is started sequentially, the purging time of each set of purifiers should not be less than 1 hour, the purging flow rate is 0.5~2 kg / h, and the purging pressure is not less than 0.5 MPa; After replacing the purifier, the initial purging time should be no less than 10 hours, the purging flow rate should be 0.5~2 kg / h, and the purging pressure should be no less than 0.5 MPa.

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