Device for producing electronic-grade carbon monoxide by utilizing cascade coupling
By using a cascaded production device and employing coupled scrubbing towers and condensation technology, the problems of high CO content and low extraction rate in distillation tail gas during the production of high-purity carbon monoxide have been solved, achieving the production of high-purity CO products with high extraction rates, meeting the standards for electronic-grade carbon monoxide.
Patent Information
- Application Number
- CN202422914406.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-27
- Publication Date
- 2025-11-21
- Estimated Expiration
- 2034-11-27
AI Technical Summary
Existing methods for producing high-purity carbon monoxide suffer from low distillation thermal efficiency and low product extraction rates. Traditional low-temperature distillation methods produce high CO content in the distillation tail gas, resulting in insufficient CO product extraction.
The cascaded production unit includes a raw material buffer tank, a raw material pretreatment unit, a light-weight distillation column, a heavy-weight distillation column, and a coupled washing column. The coupled washing column washes the gas phase of the light-weight distillation column, and combined with condensation technology, reduces the CO content in the distillation tail gas and improves the CO product extraction rate.
It achieves improved CO product extraction rate and reduced energy consumption on the basis of environmental protection. The product purity and extraction rate reach 99.999%, which meets the electronic gas carbon monoxide standard. It solves the problems of high CO content and low extraction rate in traditional methods and realizes self-sufficiency in cyclic refrigeration.
Smart Images
Figure CN223570049U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to electronic grade carbon monoxide production technical field, concretely is a device for producing electronic grade carbon monoxide by cascade coupling. BACKGROUND
[0002] Carbon monoxide as an important organic chemical raw material, can be used to prepare such as ammonia, phosgene, also can be used as reducing agent to extract high purity nickel. High purity carbon monoxide (99.99%) is mainly used in the field of semiconductor chip etching. At present, there are various methods for producing high purity carbon monoxide in China, including "synthesis gas separation and purification method", "carbon high temperature reduction carbon dioxide method", "formic acid methyl ester catalytic method", "methanol cracking method" and "formic acid dehydration method". The main industrialization technology for separating carbon monoxide from mixed gas at present is deep cooling method. The deep cooling method is mainly a high purity carbon monoxide preparation process (low temperature rectification method) using carbon monoxide tail gas as raw material. The process mainly utilizes the difference of relative volatility of each component of the raw material gas, and under low temperature conditions, the liquefied rectification is carried out in the rectification tower, and the purity of carbon monoxide can reach 99.99%. The above traditional low temperature rectification method has the problems of low rectification heat efficiency and low product extraction rate in actual operation. In the traditional rectification tower mode, the CO content in the rectification tail gas is about 25%, and the extraction rate of CO product is generally about 60%. CONTENT OF THE UTILITY MODEL
[0003] The utility model aims at providing a device for producing electronic grade carbon monoxide by cascade coupling to overcome the defects in the prior art.
[0004] To achieve the above-mentioned purpose, the utility model provides the following technical scheme:
[0005] A device for producing electronic grade carbon monoxide by cascade coupling, comprising a raw material buffer tank, the 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 removal rectification tower and a heavy removal rectification tower. The tower kettle liquid outlet at the bottom of the light removal rectification tower is connected with the inlet of the heavy removal rectification tower. A coupling washing tower is arranged at the top of the heavy removal rectification tower. The gas phase outlet at the top of the heavy removal rectification tower is connected with a washing tower reboiler at the bottom of the coupling washing tower. The outlet of the washing tower reboiler is connected with the reflux liquid port of the heavy removal rectification tower and the inlet of a product intermediate tank respectively.
[0006] The utility model discloses beneficial effect is: through setting up coupling washing tower can with rectification purification again low temperature production electron grade carbon monoxide field realizes perfect fusion, specifically speaking, the utility model discloses through the coupling washing tower to the gas phase from the light removal rectification tower and washes to reach the purpose of reducing the CO content in rectification tail gas, to realize the feature of improving the extraction rate of CO product on the basis of solving environmental protection problem, further, still can utilize the cold content in the coupling washing tower to the gas phase from the heavy removal rectification tower top and condenses, to realize the feature of saving cold content.
[0007] Preferably, the raw material pretreatment unit comprises an adsorption tower, a raw material buffer tank is connected with the adsorption tower, and the outlet of the adsorption tower is connected with the inlet of the light removal rectification tower through a first channel in a filter and a recuperator and a first valve.
[0008] Preferably, the gas phase outlet of the light removal rectification tower is connected with the lower inlet of the coupling washing tower, the lower outlet of the coupling washing tower is connected with the liquid phase reflux port of the light removal rectification tower, the top gas phase outlet of the coupling washing tower is connected with the inlet of the circulating working medium compressor through a second channel in the recuperator, the outlet of the circulating working medium compressor is connected with the first column still reboiler arranged at the bottom of the light removal rectification tower through a third channel in the recuperator, the outlet of the first column still reboiler is connected with the second column still reboiler arranged at the bottom of the heavy removal rectification tower, and the outlet of the second column still reboiler is connected with the reflux port of the upper part of the coupling washing tower through a second valve.
[0009] Preferably, the column still liquid outlet of the heavy removal rectification tower is connected with a waste gas furnace through a fourth channel in the recuperator.
[0010] Preferably, the gas phase outlet at the top of the heavy removal rectification tower is sequentially provided with a flowmeter and a third valve between the gas phase outlet and a washing tower reboiler, the outlet of the washing tower reboiler and the reflux liquid port of the heavy removal rectification tower are provided with a fourth valve, and the outlet of the washing tower reboiler and the inlet of a product intermediate tank are provided with a fifth valve.
[0011] Preferably, the rectification washing tower unit and the recuperator are arranged in a cold box.
[0012] The device for producing electronic-grade carbon monoxide by cascade coupling prepared according to the above scheme is provided with a coupling washing tower at the top of the heavy-removing rectifying tower, and a washing tower reboiler is arranged in the coupling washing tower, which provides a cold source for liquefaction of the gas at the top of the heavy-removing rectifying tower and provides reflux liquid required for rectification for the light-removing rectifying tower, further, the gas phase from the light-removing rectifying tower is washed through the coupling washing tower to reduce the CO content in the rectification tail gas, so that the feature of improving the extraction rate of the CO product on the basis of solving the environmental protection problem is realized; the flow meter and the third valve can realize control of the amount of the gas phase of the heavy-removing rectifying tower entering the coupling washing tower, and the fourth valve controls the reflux into the product intermediate tank, so as to ensure that the CO product in the product intermediate tank has a water content of ≤100ppb and a purity of ≥99.999%, and the product quality meets the standard of Electronic Gas Carbon Monoxide GB / T43771-2024; further, the gas in the coupling washing tower is used as a working medium for circulating refrigeration in the utility model, which solves the tail gas emission problem in the rectification process, and realizes the characteristics of self-sufficiency of the circulating refrigeration. BRIEF DESCRIPTION OF DRAWINGS
[0013] Figure 1 It is a structural schematic diagram of the utility model.
[0014] In the figure: 1, raw material buffer tank; 2, adsorption tower; 3, filter; 4, back cooler; 5, common tower kettle; 6, light-removing rectifying tower; 7, heavy-removing rectifying tower; 8, coupling washing tower; 9, cold box; 10, washing tower reboiler; 11, product intermediate tank; 12, circulating working medium compressor; 13, waste 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
[0015] The technical scheme in the utility model embodiment will be described clearly and completely in combination with the drawings in the utility model embodiment.
[0016] Referring to Figure 1As shown, this utility model is an apparatus for producing electronic-grade carbon monoxide using cascade coupling, including a raw material buffer tank 1. The outlet of the raw material buffer tank 1 is connected to a distillation and washing tower unit through a raw material pretreatment unit. The distillation and washing tower unit includes a light distillation tower 6 and a heavy distillation tower 7. The bottom liquid outlet of the light distillation tower 6 is connected to the inlet of the heavy distillation tower 7. A coupled washing tower 8 is provided at the top of the heavy distillation tower 7. The gas phase outlet at the top of the heavy distillation tower 7 is connected to the washing tower reboiler 10 at the bottom of the coupled washing tower 8. The outlet of the washing tower reboiler 10 is connected to the reflux liquid port of the heavy distillation tower 7 and the inlet of the product intermediate tank 11, respectively. This invention is applicable to carbon monoxide purification using distillation. Specifically, this invention couples the traditional distillation method with a coupled washing tower 8 to reduce energy consumption and increase extraction rate. The gas phase in the light distillation tower 6 enters the coupled washing tower 8 for washing, which can effectively reduce the CO content in the tail gas, thereby increasing the extraction rate. At the same time, the cooling capacity of the coupled washing tower 8 is used to condense the gas phase from the heavy distillation tower 7, thereby saving energy.
[0017] Furthermore, the raw material pretreatment unit includes an adsorption tower 2, a raw material buffer tank 1 connected to the adsorption tower 2, and the outlet of the adsorption tower 2 connected to the inlet of the light-light distillation tower 6 via a filter 3, a first channel in the cooler 4, and a first valve 15. This configuration allows for the pretreatment of the raw material in the buffer tank 1, including reducing moisture content, preliminary impurity removal, and cooling, to meet the operating requirements of the light-light distillation tower 6 and reduce the distillation load.
[0018] Furthermore, the vapor outlet of the light-weight distillation column 6 is connected to the lower inlet of the coupled washing column 8, and the lower outlet of the coupled washing column 8 is connected to the liquid reflux port of the light-weight distillation column 6. The top vapor outlet of the coupled washing column 8 is connected to the inlet of the circulating working fluid compressor 12 via a second channel in the recirculator 4. The outlet of the circulating working fluid compressor 12 is connected to the first reboiler 5 located at the bottom of the light-weight distillation column 6 via a third channel in the recirculator 4. The outlet of the first reboiler 5 is connected to the second reboiler 20 located at the bottom of the heavy-weight distillation column 7. The outlet of the second reboiler 20 is connected to the reflux port at the top of the coupled washing column 8 via a second valve 16. This configuration allows the vapor from the light-weight distillation column 6 to be used as the working fluid for circulating refrigeration, which not only solves the problem of tail gas emissions during the distillation process but also achieves self-sufficiency in circulating refrigeration, thus achieving environmental friendliness and energy conservation.
[0019] Furthermore, the bottom liquid outlet of the de-heavy distillation column 7 is connected to the waste gas furnace 13 via the fourth channel in the cooler 4. This configuration allows for the treatment of waste while recovering cooling energy.
[0020] Further, the gas phase outlet of the top of the de-heavy rectification tower 7 and the washing tower reboiler 10 are sequentially provided with a flow meter 14 and a third valve 17, the outlet of the washing tower reboiler 10 and the reflux liquid inlet of the de-heavy rectification tower 7 are provided with a fourth valve 18, and the outlet of the washing tower reboiler 10 and the inlet of the product intermediate tank 11 are provided with a fifth valve 19. Through the above arrangement, the proportion between the gas phase entering the washing tower reboiler 10 and the liquid phase refluxing to the de-heavy rectification tower 7 can be adjusted, so that the moisture content of the CO product is realized.
[0021] Further, the rectification washing tower unit and the back cooler 4 are arranged in the cold box 9. Through the above arrangement, the feature of saving energy consumption can be achieved.
[0022] The utility model also provides a production process of the device for producing electronic grade carbon monoxide by cascade coupling, which comprises the following steps:
[0023] Step one: the raw material gas in the raw material buffer tank 1 enters the de-light rectification tower 6 for rectification and purification through the adsorption tower 2, the filter 3 and the first channel in the back cooler 4 in sequence; the pressure of the raw material gas is 0.5-1.0 Mpa, the flow is 200 Nm 3 / h, the temperature is normal temperature, and the components are: CO: 25%-60%, CH4: 2%-10%, Ar: 5%-10%, N2: 20%-55% and H2O≤100 ppm; the content of the raw material gas after removing water by the adsorption tower 2 is not more than 5 ppm;
[0024] Step two: the raw material gas in the de-light rectification tower 6 in step one is continuously rectified and purified, and the light component substances in the raw material gas are removed, and the liquid phase after rectification enters the bottom of the de-light rectification tower 6; the gas phase after rectification enters the coupling washing tower 8 through the gas phase outlet at the top of the de-light rectification tower 6 for washing and purification, recovers the effective component CO in the raw material, and the raw material gas after washing by the coupling washing tower 8 is discharged through the gas phase outlet at the top of the coupling washing tower 8; the CO content in the gas passing through the gas phase outlet at the top of the de-light rectification 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 coupling washing tower 8 is not more than 5%;
[0025] Step three: the column bottom liquid of the light-removing rectifying column 6 in step two enters the heavy-removing rectifying column 7 for secondary purification rectification, the gas phase purified by the heavy-removing rectifying column 7 enters the scrubbing column reboiler 10 through the gas phase outlet at the top of the heavy-removing rectifying column 7, a flow meter 14 and a third valve 17, is condensed and liquefied in the scrubbing column reboiler 10, at this time, the carbon monoxide has been completely liquefied from gas to liquid, the liquefied carbon monoxide liquid is divided into two streams through the outlet of the scrubbing column reboiler 10, one stream enters the heavy-removing rectifying column 7 as reflux liquid through a fourth valve 18, and the other stream enters the product intermediate tank 11 for storage through a fifth valve 19; the CO product entering the product intermediate tank 11 through the fifth valve 19 has a water content of ≤100 ppb, a purity of ≥99.999%, and a product quality meeting the standard of “Electronic Gas Carbon Monoxide” GB / T 43771-2024, and the CO extraction rate is ≥85%;
[0026] Step four: the raw material gas washed by the coupling scrubbing column 8 in step two enters the second channel of the back cooler 4 and then enters the circulating working medium compressor 12 for pressurization circulation; the pressurized circulating gas enters the first column bottom reboiler 5 through the third channel in the back cooler 4 to provide heat source for the light-removing rectifying column 6, and then enters the second column bottom reboiler 20 to provide heat load for the heavy-removing rectifying column 7;
[0027] Step five: the liquid phase liquefied in step four enters the coupling scrubbing column 8 through the outlet of the second column bottom reboiler 20, a second valve 16 and the reflux inlet at the upper part of the coupling scrubbing column 8, and enters the bottom of the coupling scrubbing column 8 by gravity, and finally enters the light-removing rectifying column 6 through the lower outlet of the coupling scrubbing column 8 and the liquid phase reflux inlet of the light-removing rectifying column 6;
[0028] Step six: the liquid phase in the heavy-removing rectifying column 7 enters the waste gas furnace 13 through the fourth channel in the back cooler 4 for treatment.
[0029] The utility model discloses a cascade coupling low-temperature purification mode production electronic grade carbon monoxide, can make product carbon monoxide purity not less than 99.995%, product quality satisfies the index requirement of electronic gas carbon monoxide GB / T43771-2024, and product moisture content is less than or equal to 100ppb, far lower than national standard (moisture content is less than or equal to 1ppm) with obvious product advantage, compared with traditional rectification technology, the utility model has following advantages: 1, the perfect fusion of washing purification and rectification purification in the low-temperature production electronic grade carbon monoxide field, and the tower cauldron reboiler 20 is coupled with the coupling washing tower 8, greatly reduces the CO content in rectification tail gas (from traditional 25% reduces to 5% below), solves the environmental protection problem while improving the extraction rate of CO product (from traditional 60% improves to 85% above);2. the gas discharged from the coupling washing tower 8 is used as the working substance of circulating refrigeration, solves the rectification process tail gas emission problem, realizes the self-sufficiency of circulating refrigeration;3. the moisture index in product reduces to less than or equal to 100ppb, satisfies electronic gas carbon monoxide GB / T43771-2024 while far lower than national moisture content less than or equal to 1ppm index, satisfies the index requirement of electronic grade carbon monoxide of electronic industry, semiconductor industry, and the moisture index of electronic grade carbon monoxide of electronic industry, semiconductor industry is far lower than national standard;The utility model discloses a cold box 9 can realize the saving of cold quantity, reduce the overall land occupation of equipment and reach the characteristics of convenient movement.
[0030] Although the embodiments of the utility model have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made thereto without departing from the principles and spirit of the utility model, and the scope of the utility model is defined by the appended claims and their equivalents.
Claims
1. An apparatus for producing electronic grade carbon monoxide by means of cascade coupling, comprising a raw material buffer tank (1), characterized in that, The outlet of the raw material buffer tank (1) is connected with the rectification washing tower unit through the raw material pretreatment unit; The rectification washing tower unit comprises a light-removing rectification tower (6) and a heavy-removing rectification tower (7), the outlet of the tower kettle liquid at the bottom of the light-removing rectification tower (6) is connected with the inlet of the heavy-removing rectification tower (7), the top of the heavy-removing rectification tower (7) is provided with a coupling washing tower (8), the gas phase outlet at the top of the heavy-removing rectification tower (7) is connected with the washing tower reboiler (10) at the bottom of the coupling washing tower (8), and the outlet of the washing tower reboiler (10) is connected with the reflux liquid port of the heavy-removing rectification tower (7) and the inlet of the product intermediate tank (11) respectively.
2. The apparatus for producing electronic grade carbon monoxide using series coupling according to claim 1, wherein, The raw material pretreatment unit comprises an adsorption tower (2), the raw material buffer tank (1) is connected with the adsorption tower (2), the outlet of the adsorption tower (2) is connected with the inlet of the light-removing rectification tower (6) through the first channel in the filter (3) and the back cooler (4) and the first valve (15).
3. The apparatus for producing electronic grade carbon monoxide using series coupling according to claim 2, wherein, The gas phase outlet of the light-removing rectification tower (6) is connected with the lower inlet of the coupling washing tower (8), the lower outlet of the coupling washing tower (8) is connected with the liquid phase reflux port of the light-removing rectification tower (6), the top gas phase outlet of the coupling washing tower (8) is connected with the inlet of the circulating working medium compressor (12) through the second channel in the back cooler (4), the outlet of the circulating working medium compressor (12) is connected with the first tower kettle reboiler (5) arranged at the bottom of the light-removing rectification tower (6) through the third channel in the back cooler (4), the outlet of the first tower kettle reboiler (5) is connected with the second tower kettle reboiler (20) arranged at the bottom of the heavy-removing rectification tower (7), and the outlet of the second tower kettle reboiler (20) is connected with the reflux port of the upper part of the coupling washing tower (8) through the second valve (16).
4. The apparatus for producing electronic grade carbon monoxide using series coupling according to claim 1, wherein, The tower kettle liquid outlet of the heavy-removing rectification tower (7) is connected with the waste gas furnace (13) through the fourth channel in the back cooler (4).
5. The apparatus for producing electronic grade carbon monoxide using series coupling according to claim 2, wherein, The gas phase outlet at the top of the heavy-removing rectification tower (7) and the washing tower reboiler (10) are sequentially provided with the flow meter (14) and the third valve (17), the fourth valve (18) is arranged between the outlet of the washing tower reboiler (10) and the reflux liquid port of the heavy-removing rectification tower (7), and the 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 apparatus for producing electronic grade carbon monoxide using series coupling according to claim 2, wherein, The rectification washing tower unit and the back cooler (4) are arranged in the cold box (9).