Device for producing electronic-grade carbon monoxide by utilizing cascade coupling and production process

Abstract

The invention relates to a device for producing electronic-grade carbon monoxide by utilizing cascade coupling and a production process. Comprising a raw material buffer tank, and an outlet of the raw material buffer tank is connected with a rectification washing tower unit through a raw material pretreatment unit; the rectification washing tower unit comprises a light component removal rectifying tower and a heavy component removal rectifying tower, a tower kettle liquid outlet at the bottom of the light component removal rectifying tower is connected with an inlet of the heavy component removal rectifying tower, a coupling washing tower is arranged at the top of the heavy component removal rectifying tower, and a gas phase outlet at the top of the heavy component removal rectifying tower is connected with a washing tower reboiler at the bottom of the coupling washing tower; an outlet of the washing tower reboiler is respectively connected with a reflux liquid opening of the de-heavy rectifying tower and an inlet of the product intermediate tank; the device has the characteristics of improving the extraction rate of CO products, saving cold energy, solving the problem of tail gas emission in the rectification process and simultaneously realizing self-sufficiency of circulating refrigeration.

Description

Technical Field

[0001] The invention relates to the technical field of electronic grade carbon monoxide production, and in particular to a device and a production process for producing electronic grade carbon monoxide by utilizing cascade coupling. Background Art

[0002] Carbon monoxide, as an important organic chemical raw material, can be used to prepare ammonia, phosgene, etc., and can also be used as a reducing agent to extract high-purity nickel. High-purity carbon monoxide (99.99%) is mainly used for chip etching in the semiconductor field. At present, there are many methods for producing high-purity carbon monoxide in China, including "synthesis gas separation and purification method", "carbon high-temperature reduction of carbon dioxide method", "formic acid methyl ester catalytic method", "methanol cracking method" and "formic acid dehydration method". At present, the industrial technology for separating carbon monoxide from mixed gases is mainly cryogenic method; cryogenic method is mainly a high-purity carbon monoxide preparation process (low-temperature distillation method) using carbon monoxide-rich tail gas as raw material. This process mainly utilizes the difference in relative volatility of each component of the raw gas. Under low temperature conditions, liquefaction distillation is carried out in the distillation tower, and the purity of carbon monoxide can reach 99.99%; the above-mentioned traditional low-temperature distillation method has the problems of low distillation thermal efficiency and low product extraction rate in actual operation. In the traditional distillation tower method, the CO content in the distillation tail gas is about 25%, and the extraction rate of CO products is generally about 60%. Summary of the invention

[0003] The object of the present invention is to provide a device and a production process for producing electronic grade carbon monoxide by cascade coupling, so as to overcome the defects in the prior art.

[0004] To achieve the above object, the present invention provides the following technical solutions:

[0005] A device for producing electronic grade carbon monoxide by cascade coupling comprises a raw material buffer tank, the outlet of which is connected to a distillation washing tower unit through a raw material pretreatment unit; the distillation washing tower unit comprises a light removal distillation tower and a heavy removal distillation tower, the bottom liquid outlet of the light removal distillation tower is connected to the inlet of the heavy removal distillation tower, a coupling washing tower is arranged on the top of the heavy removal distillation tower, the gas phase outlet at the top of the heavy removal distillation tower is connected to a washing tower reboiler at the bottom of the coupling washing tower, and the outlet of the washing tower reboiler is respectively connected to the reflux liquid port of the heavy removal distillation tower and the inlet of a product intermediate tank.

[0006] The beneficial effects of the present invention are as follows: by setting up a coupled washing tower, it is possible to achieve perfect integration with the field of distillation purification and low-temperature production of electronic-grade carbon monoxide. Specifically, the present invention achieves the purpose of reducing the CO content in the distillation tail gas by washing the gas phase from the light removal distillation tower through the coupled washing tower, thereby achieving the characteristic of improving the extraction rate of CO products on the basis of solving environmental protection problems. Furthermore, the cold energy in the coupled washing tower can also be used to condense the gas phase from the top of the heavy removal distillation tower to achieve the characteristic of saving cold energy.

[0007] Preferably, the raw material pretreatment unit comprises an adsorption tower, the raw material buffer tank is connected to the adsorption tower, and the outlet of the adsorption tower is connected to the inlet of the light removal distillation tower through a filter and a first channel in a recooler and a first valve.

[0008] Preferably, the gas phase outlet of the de-lightening distillation tower is connected to the lower inlet of the coupled washing tower, the lower outlet of the coupled washing tower is connected to the liquid phase reflux port of the de-lightening distillation tower, the top gas phase outlet of the coupled washing tower is connected to the inlet of the circulating working fluid compressor through the second channel in the recooler, the outlet of the circulating working fluid compressor is connected to the first tower bottom reboiler arranged at the bottom of the de-lightening distillation tower through the third channel in the recooler, the outlet of the first tower bottom reboiler is connected to the second tower bottom reboiler arranged at the bottom of the de-heaving distillation tower, and the outlet of the second tower bottom reboiler is connected to the reflux port at the top of the coupled washing tower through the second valve.

[0009] Preferably, the bottom liquid outlet of the de-heavy distillation tower is connected to the waste gas furnace through a fourth channel in the recooler.

[0010] Preferably, a flow meter and a third valve are arranged in sequence between the gas phase outlet at the top of the de-heavy distillation tower and the reboiler of the washing tower, a fourth valve is arranged between the outlet of the washing tower reboiler and the reflux liquid port of the de-heavy distillation tower, and a fifth valve is arranged between the outlet of the washing tower reboiler and the inlet of the product intermediate tank.

[0011] Preferably, the distillation washing tower unit and the recooler are arranged in a cold box.

[0012] The present invention also provides a production process of a device for producing electronic grade carbon monoxide by cascade coupling, the process comprising the following steps:

[0013] Step 1: The raw gas in the raw material buffer tank passes through the adsorption tower, the filter and the first channel in the recooler in turn and enters the light removal distillation tower for distillation and purification; the pressure of the raw gas is 0.5-1.0Mpa and the flow rate is 200Nm 3 / h, temperature: room temperature, components: CO: 25% ~ 60%, CH4: 2% ~ 10%, Ar: 5% ~ 10%, N2: 20% ~ 55%, H2O ≤ 100ppm; the content of the raw gas after the water is removed by the adsorption tower is not more than 5ppm;

[0014] Step 2: The raw gas entering the light-removing distillation tower in step 1 is further distilled and purified, and the light components in the raw gas are removed, and the liquid phase after distillation enters the bottom of the light-removing distillation tower; the gas phase after distillation enters the coupled washing tower through the gas phase outlet at the top of the light-removing distillation tower for washing and purification, and the effective component CO in the raw material is recovered, and the raw gas washed by the coupled washing tower is discharged through the gas phase outlet at the top thereof; the CO content in the gas passing through the gas phase outlet at the top of the light-removing distillation tower is not more than 20%, and the CO content in the gas passing through the gas phase outlet at the top of the coupled washing tower is not more than 5%;

[0015] Step 3: In step 2, the bottom liquid of the de-light distillation tower enters the de-heavy distillation tower for secondary purification and distillation, and the gas phase purified by the de-heavy distillation tower enters the reboiler of the scrubbing tower through the gas phase outlet at the top of the de-heavy distillation tower through the flow meter and the third valve, and is condensed and liquefied in the reboiler of the scrubbing tower. At this time, the carbon monoxide has been completely liquefied from the gaseous state to the liquid state. The liquefied carbon monoxide liquid is divided into two streams through the outlet of the scrubbing tower reboiler, one stream enters the de-heavy distillation tower through the fourth valve as reflux liquid, and the other stream enters the product intermediate tank through the fifth valve for storage; the said de-heavy distillation tower passes through the fifth valve and enters the product intermediate tank for storage; The moisture content of the CO product entering the product intermediate tank through the valve is ≤100ppb, the purity is ≥99.999%, the product quality complies with the "Electronic Gas Carbon Monoxide" GB / T43771-2024 standard, and the CO extraction rate is ≥85%; Step 4: the raw gas after washing by the coupled washing tower in the step 2 enters the second channel of the recooler and then enters the circulating working fluid compressor for pressurized circulation; the pressurized circulating gas enters the first tower kettle reboiler through the third channel in the recooler to provide a heat source for the light degassing distillation tower, and then enters the second tower kettle reboiler to provide a heat load for the heavy degassing distillation tower;

[0016] Step 5: The liquefied liquid phase in step 4 enters the coupled washing tower through the outlet of the second tower kettle reboiler, the second valve and the reflux port at the top of the coupled washing tower, and enters the bottom of the coupled washing tower by gravity, and finally enters the light removal distillation tower through the lower outlet of the coupled washing tower and the liquid phase reflux port of the light removal distillation tower;

[0017] Step 6: The liquid phase in the deheaving distillation tower enters the waste gas furnace through the fourth channel in the recooler for treatment.

[0018] According to the above scheme, a device and production process for producing electronic grade carbon monoxide by cascade coupling is prepared. A coupled washing tower is arranged at the top of the de-heavy distillation tower. A washing tower reboiler is arranged in the coupled washing tower. On the one hand, it provides a cold source for liquefying the gas at the top of the de-heavy distillation tower, and on the other hand, it provides the reflux liquid required for distillation for the de-light distillation tower. Furthermore, the gas phase from the de-light distillation tower is washed by the coupled washing tower to achieve the purpose of reducing the CO content in the distillation tail gas, thereby achieving the characteristic of improving the extraction rate of CO products on the basis of solving environmental protection problems. The flow meter and the third valve can control the amount of gas phase from the de-heavy distillation tower entering the coupled washing tower, and cooperate with the fourth valve to control the reflux into the product intermediate tank to ensure that the moisture content of the CO product entering the product intermediate tank is ≤100ppb, the purity is ≥99.999%, and the product quality complies with the "Electronic Gas Carbon Monoxide" GB / T43771-2024 standard; further, in the present invention, the gas in the coupled washing tower is used as the working medium for circulating refrigeration, which solves the problem of tail gas emissions in the distillation process and realizes the self-sufficiency of circulating refrigeration. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a structural schematic diagram of the present invention.

[0020] In the figure: 1. raw material buffer tank; 2. adsorption tower; 3. filter; 4. recooler; 5. common tower kettle; 6. light removal distillation tower; 7. heavy removal distillation tower; 8. coupled washing tower; 9 cold box; 10. washing tower reboiler; 11. product intermediate tank; 12. circulating working fluid compressor; 13. exhaust gas furnace; 14. flow meter; 15. first valve; 16. second valve; 17. third valve; 18. fourth valve; 19. fifth valve; 20. tower kettle reboiler. DETAILED DESCRIPTION

[0021] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the accompanying drawings in the embodiments of the present invention.

[0022] Reference Figure 1As shown, the present invention is a device and production process for producing electronic grade carbon monoxide by cascade coupling, wherein the device comprises a raw material buffer tank 1, the outlet of the raw material buffer tank 1 is connected to a distillation washing tower unit through a raw material pretreatment unit; the distillation washing tower unit comprises a light removal distillation tower 6 and a heavy removal distillation tower 7, the bottom liquid outlet of the light removal distillation tower 6 is connected to the inlet of the heavy removal distillation tower 7, a coupling washing tower 8 is arranged on the top of the heavy removal distillation tower 7, the gas phase outlet at the top of the heavy removal distillation tower 7 is connected to a washing tower reboiler 10 at the bottom of the coupling washing tower 8, and the outlet of the washing tower reboiler 10 is respectively connected to the reflux liquid port of the heavy removal distillation tower 7 and the inlet of the product intermediate tank 11. The present invention is suitable for purifying carbon monoxide by distillation. Specifically, the present invention couples the traditional distillation method with the coupled washing tower 8 to achieve the characteristics of reducing energy consumption and improving the extraction rate. The gas phase in the light removal distillation tower 6 enters the coupled washing tower 8 for washing, which can effectively reduce the CO content in the tail gas and thus improve the extraction rate; at the same time, the cold capacity in the coupled washing tower 8 is used to condense the gas phase from the heavy removal distillation tower 7, thereby achieving the characteristic of saving energy consumption.

[0023] Furthermore, the raw material pretreatment unit includes an adsorption tower 2, the raw material buffer tank 1 is connected to the adsorption tower 2, and the outlet of the adsorption tower 2 is connected to the inlet of the light removal distillation tower 6 through the filter 3 and the first channel in the recooler 4 and the first valve 15. Through the above arrangement, the raw material in the raw material buffer tank 1 can be pretreated, and the pretreatment includes reducing the moisture in the raw material, preliminary impurity removal and cooling, so as to achieve the characteristics of meeting the working condition requirements of the light removal distillation tower 6 and reducing the distillation load.

[0024] Further, the gas phase outlet of the de-light fractionation tower 6 is connected to the lower inlet of the coupled washing tower 8, the lower outlet of the coupled washing tower 8 is connected to the liquid phase reflux port of the de-light fractionation tower 6, the top gas phase outlet of the coupled washing tower 8 is connected to the inlet of the circulating working fluid compressor 12 through the second channel in the recooler 4, the outlet of the circulating working fluid compressor 12 is connected to the first tower bottom reboiler 5 arranged at the bottom of the de-light fractionation tower 6 through the third channel in the recooler 4, the outlet of the first tower bottom reboiler 5 is connected to the second tower bottom reboiler 20 arranged at the bottom of the de-heavy fractionation tower 7, and the outlet of the second tower bottom reboiler 20 is connected to the reflux port at the top of the coupled washing tower 8 through the second valve 16. Through the above arrangement, the gas phase from the de-light fractionation tower 6 can be used as the working medium of the circulating refrigeration, which can not only solve the problem of tail gas emission in the distillation process, but also realize the self-sufficiency of the circulating refrigeration, so as to achieve the characteristics of environmental friendliness and energy saving and consumption reduction.

[0025] Furthermore, the bottom liquid outlet of the de-heavy distillation tower 7 is connected to the waste gas furnace 13 through the fourth channel in the recooler 4. The above arrangement can process waste while recovering cold.

[0026] Furthermore, a flow meter 14 and a third valve 17 are sequentially arranged between the gas phase outlet at the top of the de-heavy distillation tower 7 and the washing tower reboiler 10, a fourth valve 18 is arranged between the outlet of the washing tower reboiler 10 and the reflux liquid port of the de-heavy distillation tower 7, and a fifth valve 19 is arranged between the outlet of the washing tower reboiler 10 and the inlet of the product intermediate tank 11. The above arrangement can adjust the ratio between the gas phase entering the washing tower reboiler 10 and the liquid phase refluxed to the de-heavy distillation tower 7, thereby achieving the characteristics of the moisture content in the CO product.

[0027] Furthermore, the rectification and washing tower unit and the recooler 4 are arranged in the cold box 9. The above arrangement can achieve the characteristic of energy saving.

[0028] The present invention also provides a production process of a device for producing electronic grade carbon monoxide by cascade coupling, the process comprising the following steps:

[0029] Step 1: The raw gas in the raw material buffer tank 1 passes through the adsorption tower 2, the filter 3 and the first channel in the recooler 4 in turn and enters the light removal distillation tower 6 for distillation and purification; the pressure of the raw gas is 0.5-1.0Mpa and the flow rate is 200Nm 3 / h, temperature: room temperature, components: CO: 25% ~ 60%, CH4: 2% ~ 10%, Ar: 5% ~ 10%, N2: 20% ~ 55%, H2O ≤ 100ppm; the content of the raw gas after the water is removed by the adsorption tower 2 is not more than 5ppm;

[0030] Step 2: The raw gas entering the light-removing distillation tower 6 in step 1 is further distilled and purified, and the light components in the raw gas are removed, and the liquid phase after distillation enters the bottom of the light-removing distillation tower 6; the gas phase after distillation enters the coupled washing tower 8 through the gas phase outlet at the top of the light-removing distillation tower 6 for washing and purification, and the effective component CO in the raw material is recovered, and the raw gas washed by the coupled washing tower 8 is discharged through the gas phase outlet at the top thereof; the CO content in the gas passing through the gas phase outlet at the top of the light-removing distillation tower 6 is not more than 20%, and the CO content in the gas passing through the gas phase outlet at the top of the coupled washing tower 8 is not more than 5%;

[0031] Step 3: In step 2, the bottom liquid of the de-light distillation tower 6 enters the de-heavy distillation tower 7 for secondary purification and distillation. The gas phase purified by the de-heavy distillation tower 7 enters the washing tower reboiler 10 through the gas phase outlet at the top of the de-heavy distillation tower 7 through the flow meter 14 and the third valve 17, and is condensed and liquefied in the washing tower reboiler 10. At this time, the carbon monoxide has been completely liquefied from the gaseous state to the liquid state. The liquefied carbon monoxide liquid is divided into two streams through the outlet of the washing tower reboiler 10, one stream enters the de-heavy distillation tower 7 through the fourth valve 18 as a reflux liquid, and the other stream enters the product intermediate tank 11 through the fifth valve 19 for storage; the CO product moisture content entering the product intermediate tank 11 through the fifth valve 19 is ≤100ppb, the purity is ≥99.999%, the product quality meets the "Electronic Gas Carbon Monoxide" GB / T43771-2024 standard, and the CO extraction rate is ≥85%;

[0032] Step 4: the raw gas washed by the coupled washing tower 8 in the step 2 enters the second channel of the recooler 4 and then enters the circulating working fluid compressor 12 for pressurization circulation; the pressurized circulating gas enters the first tower kettle reboiler 5 through the third channel in the recooler 4 to provide a heat source for the light removal distillation tower 6, and then enters the second tower kettle reboiler 20 to provide a heat load for the heavy removal distillation tower 7;

[0033] Step 5: The liquefied liquid phase in step 4 enters the coupled washing tower 8 through the outlet of the second tower kettle reboiler 20, the second valve 16 and the reflux port at the top of the coupled washing tower 8, and enters the bottom of the coupled washing tower 8 by gravity, and finally enters the light removal distillation tower 6 through the lower outlet of the coupled washing tower 8 and the liquid phase reflux port of the light removal distillation tower 6;

[0034] Step 6: The liquid phase in the de-heavy distillation tower 7 enters the waste gas furnace 13 through the fourth channel in the recooler 4 for treatment.

[0035] The present invention adopts a cascade-coupled low-temperature purification method to produce electronic-grade carbon monoxide, which can make the purity of the product carbon monoxide not less than 99.995%, and the product quality meets the index requirements of "Electronic Gas Carbon Monoxide" GB / T43771-2024, and the product moisture content is ≤100ppb, which is far lower than the national standard (water content ≤1ppm) and has obvious product advantages; compared with traditional distillation technology, the present invention has the following advantages: 1. The washing purification and distillation purification are perfectly integrated in the field of low-temperature production of electronic-grade carbon monoxide, and the tower kettle reboiler 20 is coupled with the coupled washing tower 8, which greatly reduces the distillation tail 1. The CO content in the gas (reduced from the traditional 25% to less than 5%), while solving environmental problems, the extraction rate of CO products is improved (increased from the traditional 60% to more than 85%); 2. The gas discharged from the coupling washing tower 8 is used as the working medium of the circulating refrigeration, which solves the problem of tail gas emissions in the distillation process and realizes the self-sufficiency of the circulating refrigeration; 3. The moisture index in the product is reduced to less than 100ppb, and the quality meets the "Electronic Gas Carbon Monoxide" GB / T43771-2024, while being far lower than the national water content ≤1ppm index, meeting the index requirements of the electronics industry and the semiconductor industry for electronic-grade carbon monoxide. The water index of the electronics industry and the semiconductor industry for electronic-grade carbon monoxide is far lower than the national standard; the present invention can save cooling capacity, reduce the overall footprint of the equipment, and achieve the characteristics of easy mobility by setting a cold box 9.

[0036] In order to explain the present invention in more detail, the present invention is further described in conjunction with embodiments. The specific embodiments are as follows:

[0037] Example 1

[0038] The present invention is a device for producing electronic grade carbon monoxide by cascade coupling, comprising a raw material buffer tank 1, the outlet of the raw material buffer tank 1 is connected to a distillation washing tower unit through a raw material pretreatment unit; the distillation washing tower unit comprises a light removal distillation tower 6 and a heavy removal distillation tower 7, the tower bottom liquid outlet at the bottom of the light removal distillation tower 6 is connected to the inlet of the heavy removal distillation tower 7, a coupling washing tower 8 is arranged at the top of the heavy removal distillation tower 7, the gas phase outlet at the top of the heavy removal distillation tower 7 is connected to a washing tower reboiler 10 at the bottom of the coupling washing tower 8, and the outlet of the washing tower reboiler 10 is respectively connected to the reflux liquid port of the heavy removal distillation tower 7 and the inlet of the product intermediate tank 11. The raw material pretreatment unit comprises an adsorption tower 2, the raw material buffer tank 1 is connected to the adsorption tower 2, and the outlet of the adsorption tower 2 is connected to the inlet of the light removal distillation tower 6 through a filter 3 and a first channel in a recooler 4 and a first valve 15. The gas phase outlet of the de-light distillation tower 6 is connected to the lower inlet of the coupled washing tower 8, the lower outlet of the coupled washing tower 8 is connected to the liquid phase reflux port of the de-light distillation tower 6, the top gas phase outlet of the coupled washing tower 8 is connected to the inlet of the circulating working fluid compressor 12 through the second channel in the recooler 4, the outlet of the circulating working fluid compressor 12 is connected to the first tower bottom reboiler 5 arranged at the bottom of the de-light distillation tower 6 through the third channel in the recooler 4, the outlet of the first tower bottom reboiler 5 is connected to the second tower bottom reboiler 20 arranged at the bottom of the de-heavy distillation tower 7, and the outlet of the second tower bottom reboiler 20 is connected to the reflux port at the top of the coupled washing tower 8 through the second valve 16. The tower bottom liquid outlet of the de-heavy distillation tower 7 is connected to the exhaust gas furnace 13 through the fourth channel in the recooler 4. A flow meter 14 and a third valve 17 are sequentially arranged between the gas phase outlet at the top of the de-heavy distillation tower 7 and the washing tower reboiler 10, a fourth valve 18 is arranged between the outlet of the washing tower reboiler 10 and the reflux liquid port of the de-heavy distillation tower 7, and a fifth valve 19 is arranged between the outlet of the washing tower reboiler 10 and the inlet of the product intermediate tank 11. The distillation washing tower unit and the recooler 4 are arranged in a cold box 9.

[0039] The present invention also provides a production process of a device for producing electronic grade carbon monoxide by cascade coupling, the process comprising the following steps:

[0040] Step 1: The raw gas in the raw material buffer tank 1 passes through the adsorption tower 2, the filter 3 and the first channel in the recooler 4 in turn and enters the light removal distillation tower 6 for distillation and purification; the pressure of the raw gas is 0.5-1.0Mpa and the flow rate is 200Nm 3 / h, temperature: room temperature, components: CO: 25% ~ 60%, CH4: 2% ~ 10%, Ar: 5% ~ 10%, N2: 20% ~ 55%, H2O ≤ 100ppm; the content of the raw gas after the water is removed by the adsorption tower 2 is not more than 5ppm;

[0041] Step 2: The raw gas entering the light-removing distillation tower 6 in step 1 is further distilled and purified, and the light components in the raw gas are removed, and the liquid phase after distillation enters the bottom of the light-removing distillation tower 6; the gas phase after distillation enters the coupled washing tower 8 through the gas phase outlet at the top of the light-removing distillation tower 6 for washing and purification, and the effective component CO in the raw material is recovered. The raw gas washed by the coupled washing tower 8 is discharged through the gas phase outlet at the top thereof; the CO content in the gas passing through the gas phase outlet at the top of the light-removing distillation tower 6 is 20%, and the CO content in the gas passing through the gas phase outlet at the top of the coupled washing tower 8 is 5%;

[0042] Step 3: In step 2, the bottom liquid of the de-light distillation tower 6 enters the de-heavy distillation tower 7 for secondary purification and distillation. The gas phase purified by the de-heavy distillation tower 7 enters the washing tower reboiler 10 through the gas phase outlet at the top of the de-heavy distillation tower 7 through the flow meter 14 and the third valve 17, and is condensed and liquefied in the washing tower reboiler 10. At this time, the carbon monoxide has been completely liquefied from the gaseous state to the liquid state. The liquefied carbon monoxide liquid is divided into two streams through the outlet of the washing tower reboiler 10, one stream enters the de-heavy distillation tower 7 through the fourth valve 18 as a reflux liquid, and the other stream enters the product intermediate tank 11 through the fifth valve 19 for storage; the CO product moisture content entering the product intermediate tank 11 through the fifth valve 19 is ≤100ppb, the purity is ≥99.999%, the product quality meets the "Electronic Gas Carbon Monoxide" GB / T43771-2024 standard, and the CO extraction rate is ≥85%;

[0043] Step 4: the raw gas washed by the coupled washing tower 8 in the step 2 enters the second channel of the recooler 4 and then enters the circulating working fluid compressor 12 for pressurization circulation; the pressurized circulating gas enters the first tower kettle reboiler 5 through the third channel in the recooler 4 to provide a heat source for the light removal distillation tower 6, and then enters the second tower kettle reboiler 20 to provide a heat load for the heavy removal distillation tower 7;

[0044] Step 5: The liquefied liquid phase in step 4 enters the coupled washing tower 8 through the outlet of the second tower kettle reboiler 20, the second valve 16 and the reflux port at the top of the coupled washing tower 8, and enters the bottom of the coupled washing tower 8 by gravity, and finally enters the light removal distillation tower 6 through the lower outlet of the coupled washing tower 8 and the liquid phase reflux port of the light removal distillation tower 6;

[0045] Step 6: The liquid phase in the de-heavy distillation tower 7 enters the waste gas furnace 13 through the fourth channel in the recooler 4 for treatment.

[0046] Example 2

[0047] The present invention is a device for producing electronic grade carbon monoxide by cascade coupling, comprising a raw material buffer tank 1, the outlet of the raw material buffer tank 1 is connected to a distillation washing tower unit through a raw material pretreatment unit; the distillation washing tower unit comprises a light removal distillation tower 6 and a heavy removal distillation tower 7, the tower bottom liquid outlet at the bottom of the light removal distillation tower 6 is connected to the inlet of the heavy removal distillation tower 7, a coupling washing tower 8 is arranged at the top of the heavy removal distillation tower 7, the gas phase outlet at the top of the heavy removal distillation tower 7 is connected to a washing tower reboiler 10 at the bottom of the coupling washing tower 8, and the outlet of the washing tower reboiler 10 is respectively connected to the reflux liquid port of the heavy removal distillation tower 7 and the inlet of the product intermediate tank 11. The raw material pretreatment unit comprises an adsorption tower 2, the raw material buffer tank 1 is connected to the adsorption tower 2, and the outlet of the adsorption tower 2 is connected to the inlet of the light removal distillation tower 6 through a filter 3 and a first channel in a recooler 4 and a first valve 15. The gas phase outlet of the de-light distillation tower 6 is connected to the lower inlet of the coupled washing tower 8, the lower outlet of the coupled washing tower 8 is connected to the liquid phase reflux port of the de-light distillation tower 6, the top gas phase outlet of the coupled washing tower 8 is connected to the inlet of the circulating working fluid compressor 12 through the second channel in the recooler 4, the outlet of the circulating working fluid compressor 12 is connected to the first tower bottom reboiler 5 arranged at the bottom of the de-light distillation tower 6 through the third channel in the recooler 4, the outlet of the first tower bottom reboiler 5 is connected to the second tower bottom reboiler 20 arranged at the bottom of the de-heavy distillation tower 7, and the outlet of the second tower bottom reboiler 20 is connected to the reflux port at the top of the coupled washing tower 8 through the second valve 16. The tower bottom liquid outlet of the de-heavy distillation tower 7 is connected to the exhaust gas furnace 13 through the fourth channel in the recooler 4. A flow meter 14 and a third valve 17 are sequentially arranged between the gas phase outlet at the top of the de-heavy distillation tower 7 and the washing tower reboiler 10, a fourth valve 18 is arranged between the outlet of the washing tower reboiler 10 and the reflux liquid port of the de-heavy distillation tower 7, and a fifth valve 19 is arranged between the outlet of the washing tower reboiler 10 and the inlet of the product intermediate tank 11. The distillation washing tower unit and the recooler 4 are arranged in a cold box 9.

[0048] The present invention also provides a production process of a device for producing electronic grade carbon monoxide by cascade coupling, the process comprising the following steps:

[0049] Step 1: The raw gas in the raw material buffer tank 1 passes through the adsorption tower 2, the filter 3 and the first channel in the recooler 4 in turn and enters the light removal distillation tower 6 for distillation and purification; the pressure of the raw gas is 0.5-1.0Mpa and the flow rate is 200Nm 3 / h, temperature: room temperature, components: CO: 25% ~ 60%, CH4: 2% ~ 10%, Ar: 5% ~ 10%, N2: 20% ~ 55%, H2O ≤ 100ppm; the content of the raw gas after the water is removed by the adsorption tower 2 is not more than 5ppm;

[0050] Step 2: The raw gas entering the light-removing distillation tower 6 in step 1 is further distilled and purified, and the light components in the raw gas are removed, and the liquid phase after distillation enters the bottom of the light-removing distillation tower 6; the gas phase after distillation enters the coupled washing tower 8 through the gas phase outlet at the top of the light-removing distillation tower 6 for washing and purification, and the effective component CO in the raw material is recovered. The raw gas washed by the coupled washing tower 8 is discharged through the gas phase outlet at the top thereof; the CO content in the gas passing through the gas phase outlet at the top of the light-removing distillation tower 6 is 18%, and the CO content in the gas passing through the gas phase outlet at the top of the coupled washing tower 8 is 4.5%;

[0051] Step 3: In step 2, the bottom liquid of the de-light distillation tower 6 enters the de-heavy distillation tower 7 for secondary purification and distillation. The gas phase purified by the de-heavy distillation tower 7 enters the washing tower reboiler 10 through the gas phase outlet at the top of the de-heavy distillation tower 7 through the flow meter 14 and the third valve 17, and is condensed and liquefied in the washing tower reboiler 10. At this time, the carbon monoxide has been completely liquefied from the gaseous state to the liquid state. The liquefied carbon monoxide liquid is divided into two streams through the outlet of the washing tower reboiler 10, one stream enters the de-heavy distillation tower 7 through the fourth valve 18 as a reflux liquid, and the other stream enters the product intermediate tank 11 through the fifth valve 19 for storage; the CO product moisture content entering the product intermediate tank 11 through the fifth valve 19 is ≤100ppb, the purity is ≥99.999%, the product quality meets the "Electronic Gas Carbon Monoxide" GB / T43771-2024 standard, and the CO extraction rate is ≥85%;

[0052] Step 4: the raw gas washed by the coupled washing tower 8 in the step 2 enters the second channel of the recooler 4 and then enters the circulating working fluid compressor 12 for pressurization circulation; the pressurized circulating gas enters the first tower kettle reboiler 5 through the third channel in the recooler 4 to provide a heat source for the light removal distillation tower 6, and then enters the second tower kettle reboiler 20 to provide a heat load for the heavy removal distillation tower 7;

[0053] Step 5: The liquefied liquid phase in step 4 enters the coupled washing tower 8 through the outlet of the second tower kettle reboiler 20, the second valve 16 and the reflux port at the top of the coupled washing tower 8, and enters the bottom of the coupled washing tower 8 by gravity, and finally enters the light removal distillation tower 6 through the lower outlet of the coupled washing tower 8 and the liquid phase reflux port of the light removal distillation tower 6;

[0054] Step 6: The liquid phase in the de-heavy distillation tower 7 enters the waste gas furnace 13 through the fourth channel in the recooler 4 for treatment.

[0055] Example 3

[0056] The present invention is a device for producing electronic grade carbon monoxide by cascade coupling, comprising a raw material buffer tank 1, the outlet of the raw material buffer tank 1 is connected to a distillation washing tower unit through a raw material pretreatment unit; the distillation washing tower unit comprises a light removal distillation tower 6 and a heavy removal distillation tower 7, the tower bottom liquid outlet at the bottom of the light removal distillation tower 6 is connected to the inlet of the heavy removal distillation tower 7, a coupling washing tower 8 is arranged at the top of the heavy removal distillation tower 7, the gas phase outlet at the top of the heavy removal distillation tower 7 is connected to a washing tower reboiler 10 at the bottom of the coupling washing tower 8, and the outlet of the washing tower reboiler 10 is respectively connected to the reflux liquid port of the heavy removal distillation tower 7 and the inlet of the product intermediate tank 11. The raw material pretreatment unit comprises an adsorption tower 2, the raw material buffer tank 1 is connected to the adsorption tower 2, and the outlet of the adsorption tower 2 is connected to the inlet of the light removal distillation tower 6 through a filter 3 and a first channel in a recooler 4 and a first valve 15. The gas phase outlet of the de-light distillation tower 6 is connected to the lower inlet of the coupled washing tower 8, the lower outlet of the coupled washing tower 8 is connected to the liquid phase reflux port of the de-light distillation tower 6, the top gas phase outlet of the coupled washing tower 8 is connected to the inlet of the circulating working fluid compressor 12 through the second channel in the recooler 4, the outlet of the circulating working fluid compressor 12 is connected to the first tower bottom reboiler 5 arranged at the bottom of the de-light distillation tower 6 through the third channel in the recooler 4, the outlet of the first tower bottom reboiler 5 is connected to the second tower bottom reboiler 20 arranged at the bottom of the de-heavy distillation tower 7, and the outlet of the second tower bottom reboiler 20 is connected to the reflux port at the top of the coupled washing tower 8 through the second valve 16. The tower bottom liquid outlet of the de-heavy distillation tower 7 is connected to the exhaust gas furnace 13 through the fourth channel in the recooler 4. A flow meter 14 and a third valve 17 are sequentially arranged between the gas phase outlet at the top of the de-heavy distillation tower 7 and the washing tower reboiler 10, a fourth valve 18 is arranged between the outlet of the washing tower reboiler 10 and the reflux liquid port of the de-heavy distillation tower 7, and a fifth valve 19 is arranged between the outlet of the washing tower reboiler 10 and the inlet of the product intermediate tank 11. The distillation washing tower unit and the recooler 4 are arranged in a cold box 9.

[0057] The present invention also provides a production process of a device for producing electronic grade carbon monoxide by cascade coupling, the process comprising the following steps:

[0058] Step 1: The raw gas in the raw material buffer tank 1 passes through the adsorption tower 2, the filter 3 and the first channel in the recooler 4 in turn and enters the light removal distillation tower 6 for distillation and purification; the pressure of the raw gas is 0.5-1.0Mpa and the flow rate is 200Nm 3 / h, temperature: room temperature, components: CO: 25% ~ 60%, CH4: 2% ~ 10%, Ar: 5% ~ 10%, N2: 20% ~ 55%, H2O ≤ 100ppm; the content of the raw gas after the water is removed by the adsorption tower 2 is not more than 5ppm;

[0059] Step 2: The raw gas entering the de-lightening distillation tower 6 in step 1 is further distilled and purified, and the light components in the raw gas are removed, and the liquid phase after distillation enters the bottom of the de-lightening distillation tower 6; the gas phase after distillation enters the coupled washing tower 8 through the gas phase outlet at the top of the de-lightening distillation tower 6 for washing and purification, and the effective component CO in the raw material is recovered. The raw gas washed by the coupled washing tower 8 is discharged through the gas phase outlet at the top thereof; the CO content in the gas passing through the gas phase outlet at the top of the de-lightening distillation tower 6 is 17%, and the CO content in the gas passing through the gas phase outlet at the top of the coupled washing tower 8 is 4%;

[0060] Step 3: In step 2, the bottom liquid of the de-light distillation tower 6 enters the de-heavy distillation tower 7 for secondary purification and distillation. The gas phase purified by the de-heavy distillation tower 7 enters the washing tower reboiler 10 through the gas phase outlet at the top of the de-heavy distillation tower 7 through the flow meter 14 and the third valve 17, and is condensed and liquefied in the washing tower reboiler 10. At this time, the carbon monoxide has been completely liquefied from the gaseous state to the liquid state. The liquefied carbon monoxide liquid is divided into two streams through the outlet of the washing tower reboiler 10, one stream enters the de-heavy distillation tower 7 through the fourth valve 18 as a reflux liquid, and the other stream enters the product intermediate tank 11 through the fifth valve 19 for storage; the CO product moisture content entering the product intermediate tank 11 through the fifth valve 19 is ≤100ppb, the purity is ≥99.999%, the product quality meets the "Electronic Gas Carbon Monoxide" GB / T43771-2024 standard, and the CO extraction rate is ≥85%;

[0061] Step 4: the raw gas washed by the coupled washing tower 8 in the step 2 enters the second channel of the recooler 4 and then enters the circulating working fluid compressor 12 for pressurization circulation; the pressurized circulating gas enters the first tower kettle reboiler 5 through the third channel in the recooler 4 to provide a heat source for the light removal distillation tower 6, and then enters the second tower kettle reboiler 20 to provide a heat load for the heavy removal distillation tower 7;

[0062] Step 5: The liquefied liquid phase in step 4 enters the coupled washing tower 8 through the outlet of the second tower kettle reboiler 20, the second valve 16 and the reflux port at the top of the coupled washing tower 8, and enters the bottom of the coupled washing tower 8 by gravity, and finally enters the light removal distillation tower 6 through the lower outlet of the coupled washing tower 8 and the liquid phase reflux port of the light removal distillation tower 6;

[0063] Step 6: The liquid phase in the de-heavy distillation tower 7 enters the waste gas furnace 13 through the fourth channel in the recooler 4 for treatment.

[0064] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A device for producing electronic grade carbon monoxide by cascade coupling, comprising a raw material buffer tank (1), characterized in that: The outlet of the raw material buffer tank (1) is connected to the distillation washing tower unit through the raw material pretreatment unit; The distillation and washing tower unit comprises a light removal distillation tower (6) and a heavy removal distillation tower (7), wherein the bottom liquid outlet of the light removal distillation tower (6) is connected to the inlet of the heavy removal distillation tower (7), and a coupling washing tower (8) is arranged at the top of the heavy removal distillation tower (7), wherein the gas phase outlet at the top of the heavy removal distillation tower (7) is connected to a washing tower reboiler (10) at the bottom of the coupling washing tower (8), and the outlet of the washing tower reboiler (10) is respectively connected to the reflux liquid port of the heavy removal distillation tower (7) and the inlet of the product intermediate tank (11).

2. The device for producing electronic grade carbon monoxide by cascade coupling according to claim 1, characterized in that: The raw material pretreatment unit comprises an adsorption tower (2), a raw material buffer tank (1) connected to the adsorption tower (2), and an outlet of the adsorption tower (2) connected to an inlet of a light fractionation tower (6) via a filter (3) and a first channel in a recooler (4) and a first valve (15).

3. The device for producing electronic grade carbon monoxide by cascade coupling according to claim 2, characterized in that: The gas phase outlet of the de-light fractionation tower (6) is connected to the lower inlet of the coupled washing tower (8), the lower outlet of the coupled washing tower (8) is connected to the liquid phase reflux port of the de-light fractionation tower (6), the top gas phase outlet of the coupled washing tower (8) is connected to the inlet of the circulating working fluid compressor (12) through the second channel in the recooler (4), the outlet of the circulating working fluid compressor (12) is connected to the first tower kettle reboiler (5) arranged at the bottom of the de-light fractionation tower (6) through the third channel in the recooler (4), the outlet of the first tower kettle reboiler (5) is connected to the second tower kettle reboiler (20) arranged at the bottom of the de-heavy fractionation tower (7), and the outlet of the second tower kettle reboiler (20) is connected to the reflux port at the top of the coupled washing tower (8) through the second valve (16).

4. The device for producing electronic grade carbon monoxide by cascade coupling according to claim 1, characterized in that: The bottom liquid outlet of the de-heavy distillation tower (7) is connected to the waste gas furnace (13) through the fourth channel in the recooler (4).

5. The device for producing electronic grade carbon monoxide by cascade coupling according to claim 2, characterized in that: A flow meter (14) and a third valve (17) are arranged in sequence between the gas phase outlet at the top of the de-heavy distillation tower (7) and the washing tower reboiler (10), a fourth valve (18) is arranged between the outlet of the washing tower reboiler (10) and the reflux liquid port of the de-heavy distillation tower (7), and a fifth valve (19) is arranged between the outlet of the washing tower reboiler (10) and the inlet of the product intermediate tank (11).

6. The device for producing electronic grade carbon monoxide by cascade coupling according to claim 2, characterized in that: The distillation washing tower unit and the recooler (4) are arranged in a cold box (9).

7. A production process for a device for producing electronic grade carbon monoxide using cascade coupling, characterized in that: The process includes the following steps: Step 1: The raw gas in the raw material buffer tank (1) passes through the adsorption tower (2), the filter (3) and the first channel in the recooler (4) in sequence and enters the light removal distillation tower (6) for distillation and purification; the pressure of the raw gas is 0.5-1.0Mpa and the flow rate is 200Nm 3 / h, temperature: room temperature, components: CO: 25% to 60%, CH4: 2% to 10%, Ar: 5% to 10%, N2: 20% to 55%, H2O ≤ 100ppm; the content of the raw gas after water removal by the adsorption tower (2) is no more than 5ppm; Step 2: the raw gas entering the de-lightening distillation tower (6) in step 1 is further distilled and purified, and the light components in the raw gas are removed, and the liquid phase after distillation enters the bottom of the de-lightening distillation tower (6); the gas phase after distillation enters the coupled washing tower (8) through the gas phase outlet at the top of the de-lightening distillation tower (6) for washing and purification, and the effective component CO in the raw material is recovered, and the raw gas washed by the coupled washing tower (8) is discharged through the gas phase outlet at the top thereof; the CO content in the gas passing through the gas phase outlet at the top of the de-lightening distillation tower (6) is not more than 20%, and the CO content in the gas passing through the gas phase outlet at the top of the coupled washing tower (8) is not more than 5%; Step 3: The bottom liquid of the de-light distillation tower (6) in step 2 enters the de-heavy distillation tower (7) for secondary purification and distillation. The gas phase purified by the de-heavy distillation tower (7) enters the washing tower reboiler (10) through the gas phase outlet at the top of the de-heavy distillation tower (7) through the flow meter (14) and the third valve (17). The gas phase is condensed and liquefied in the washing tower reboiler (10). At this time, the carbon monoxide is completely liquefied from the gaseous state to the liquid state. The liquefied carbon monoxide liquid passes through the washing tower reboiler ( The outlet of 10) is divided into two streams, one stream is used as reflux liquid and enters the de-weighting distillation tower (7) through the fourth valve (18), and the other stream is stored in the product intermediate tank (11) through the fifth valve (19); the CO product entering the product intermediate tank (11) through the fifth valve (19) has a moisture content of ≤100ppb and a purity of ≥99.999%, and the product quality complies with the standard of "Electronic Gas Carbon Monoxide" GB / T43771-2024, and the CO extraction rate is ≥85%; Step 4: the raw gas washed by the coupled washing tower (8) in the step 2 enters the second channel of the recooler (4) and then enters the circulating working fluid compressor (12) for pressurized circulation; the pressurized circulating gas enters the first tower kettle reboiler (5) through the third channel in the recooler (4) to provide a heat source for the light removal distillation tower (6), and then enters the second tower kettle reboiler (20) to provide a heat load for the heavy removal distillation tower (7); Step 5: the liquefied liquid phase in step 4 enters the coupled washing tower (8) through the outlet of the second tower kettle reboiler (20), the second valve (16) and the reflux port at the top of the coupled washing tower (8), and enters the bottom of the coupled washing tower (8) by gravity, and finally enters the light removal distillation tower (6) through the lower outlet of the coupled washing tower (8) and the liquid phase reflux port of the light removal distillation tower (6); Step 6: The liquid phase in the de-heavy distillation tower (7) enters the waste gas furnace (13) through the fourth channel in the recooler (4) for treatment.

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