Method for cryogenically separating air and distillation column system suitable therefor
The dual-column side-by-side arrangement with optimized condenser evaporator and pressure-reducing devices, along with a gas-liquid separator and subcooler, addresses yield and cost challenges in cryogenic air separation, improving nitrogen extraction and reducing equipment costs.
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- LAIR LIQUIDE SA POUR LETUDE & LEXPLOITATION DES PROCEDES GEORGES CLAUDE
- Filing Date
- 2025-11-13
- Publication Date
- 2026-06-04
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Figure CN2025134635_04062026_PF_FP_ABST
Abstract
Description
METHOD FOR CRYOGENICALLY SEPARATING AIR AND DISTILLATION COLUMN SYSTEM SUITABLE THEREFORTECHNICAL FIELD
[0001] The present invention belongs to the field of air separation, relates to a cryogenic air separation apparatus and separation method, and particularly relates to a dual-column distillation apparatus and distillation method with a side-by-side arrangement.BACKGROUND ART
[0002] Producing air products such as oxygen, nitrogen, and argon by cryogenically rectifying air is a known technology. A cryogenic rectification air separation apparatus generally includes a main air compressor, an air precooling and purification system, a main heat exchanger, and a distillation column system.
[0003] The design and arrangement of the distillation column system therein not only determine the purity and yield of products, but also affect the manufacturing cost and operating cost of the apparatus.
[0004] If the product of cryogenic distillation is mainly nitrogen, and the concentrated oxygen is discharged as part of waste gas, such an apparatus is also called a nitrogen generator. A nitrogen generator may be single-column or multi-column.
[0005] US 4, 222, 756 discloses a conventional nitrogen-producing dual-column cycle, in which a low-pressure column is stacked on top of a high-pressure column.
[0006] Condenser evaporators are placed at the top of the low-pressure column and the top of the high-pressure column, respectively. Nitrogen gas from the low-pressure column is withdrawn as a product, and nitrogen gas from the high-pressure column is expanded to generate the cooling capacity required by the system.
[0007] US 4, 453, 957 discloses a similar apparatus, but the nitrogen produced by both the high-pressure column and the low-pressure column is withdrawn as product, and other liquid streams are expanded to generate the cooling capacity required by the system.
[0008] US 4, 717, 410 discloses a dual-column nitrogen generator, in which a low-pressure column is stacked on top of a high-pressure column. Condenser evaporators are installed at the tops of the high-pressure column and the low-pressure column, respectively. A part of the liquid nitrogen obtained at the top of the low-pressure column is pressurized and fed to the high-pressure column as a partial reflux liquid, increasing the yield of high-pressure nitrogen gas.
[0009] CN 217737679U discloses a distillation system with a side-by-side dual-column arrangement, in which condenser evaporators are installed at the tops of the high-pressure column and the low-pressure column, respectively, and the oxygen-rich liquid air from the bottom of each column is fed to the condenser evaporator at the top of that column to be vaporized.
[0010] CN 212006434U discloses a distillation system with a side-by-side dual-column arrangement, in which condenser evaporators are installed at the tops of the high-pressure column and the low-pressure column, respectively. Oxygen-rich liquid air from the bottom of the high-pressure column is transferred to the condenser evaporator at the top of that column to be vaporized, and oxygen-rich liquid air from the bottom of the low-pressure column and a bottom liquid from the condenser evaporator of the high-pressure column are transferred to the condenser evaporator at the top of the low-pressure column to be vaporized. Low-pressure liquid nitrogen obtained by condensation in the low-pressure column condenser evaporator is pressurized by a liquid nitrogen pump and sent back to the top of the high-pressure column as a reflux liquid, so as to increase the yie ld of the high-pressure column nitrogen gas product.
[0011] It can be seen from the above patents that if a stacked arrangement of two columns is adopted, the height difference can often be used to transport streams, thereby avoiding the use of liquid pumps and reducing the investment and maintenance costs of the equipment; however, when the height of the entire column and the height of the insulated cold box surrounding the column are excessive, difficulties in manufacturing, transportation, installation, and operation will arise. If a side-by-side arrangement of two columns is adopted, one or more liquid pumps are required, which increases the cost. Therefore, reducing equipment investment while increasing the nitrogen extraction rate is a problem to be solved by those skilled in the art.SUMMARY OF THE INVENTION
[0012] The present invention aims to provide a cryogenic air separation method and a distillation column system suitable for the method, so as to overcome the technical problems mentioned above and achieve the objectives of optimizing yield and reducing investment.
[0013] To achieve the above inventive objective, in one aspect, the present invention discloses a method for cryogenically separating air.
[0014] The equipment required for this method includes a main air compressor, an air precooling and purification system, a main heat exchanger, and a distillation column system. The distillation column system comprises at least one high-pressure column and one low-pressure column, a first condenser evaporator and a second condenser evaporator, a first pressure-reducing device, a second pressure-reducing device, a third pressure-reducing device, at least one liquid nitrogen pump, and at least one gas-liquid separator.
[0015] A feed air, after being compressed by the main air compressor, is precooled, and purified, and then is heat-exchanged and liquefied in the main heat exchanger with a return stream from the distillation column system, and then fed into a lower part of the high-pressure column; the feed air is rectified in the high-pressure column to produce a high-pressure column bottom oxygen-rich stream at a bottom of the high-pressure column and to produce a high-pressure nitrogen-rich vapor at a top of the high-pressure column. At least a part of the high-pressure column bottom oxygen-rich stream is reduced in pressure via the first pressure-reducing device and fed into the low-pressure column arranged substantially side-by-side, and is rectified in the low-pressure column to produce a low-pressure column bottom oxygen-rich stream at a bottom of the low-pressure column and to produce a low-pressure nitrogen-rich vapor at a top of the low-pressure column. The first condenser evaporator, provided at the bottom of the low-pressure column, receives the high-pressure nitrogen-rich vapor from the top of the high-pressure column and heat exchanges it with the low-pressure column bottom oxygen-rich stream, to condense the high-pressure nitrogen-rich vapor to obtain a high-pressure liquid nitrogen, and to partially evaporate the low-pressure column bottom oxygen-rich stream to generate a first condenser evaporator bottom liquid. The second condenser evaporator, disposed at an upper part of the low-pressure column, receives the low-pressure nitrogen-rich vapor from the top of the low-pressure column and heat exchanges it with the first condenser evaporator bottom liquid that has been reduced in pressure via the second pressure-reducing device. The low-pressure nitrogen-rich vapor is condensed to obtain a low-pressure liquid nitrogen, at least a first portion of the low-pressure liquid nitrogen serving as a low-pressure column reflux liquid; the first condenser evaporator bottom liquid is partially evaporated to generate an oxygen-rich waste gas stream and is discharged. At least a part of the high-pressure liquid nitrogen is reduced in pressure via the third pressure-reducing device and fed into the gas-liquid separator, wherein a gas phase separated therein is sent back to an upper part of the low-pressure column, and a liquid phase separated therein is pressurized by the liquid nitrogen pump and then fed into the high-pressure column as a high-pressure column reflux liquid. The low-pressure liquid nitrogen further comprises a second portion of low-pressure liquid nitrogen, the second portion of low-pressure liquid nitrogen merges with the liquid phase from the gas-liquid separator, is pressurized by the liquid nitrogen pump, and then fed into the high-pressure column as the high-pressure column reflux liquid. Streams such as the oxygen-rich waste gas stream, the high-pressure nitrogen gas product, and even parts of the low-pressure liquid nitrogen and the high-pressure liquid nitrogen are all cryogenic streams. As needed, these streams can be sent back to the main heat exchanger as return streams to cool and liquefy the feed air.
[0016] Preferably, the method of the present invention further comprises the step of sending a flash gas generated downstream of the liquid nitrogen pump back to the gas-liquid separator.
[0017] Further, the method of the present invention further comprises a subcooler. The high-pressure column reflux liquid, before returning to the high-pressure column, indirectly heat exchanges with the high-pressure liquid nitrogen in the subcooler, and the subcooled high-pressure liquid nitrogen is reduced in pressure via the third pressure-reducing device and then fed into the gas-liquid separator.
[0018] In another aspect, the present invention discloses a distillation column system suitable for the foregoing method, the system comprising at least one high-pressure column and one low-pressure column, a first condenser evaporator and a second condenser evaporator, a first pressure-reducing device, a second pressure-reducing device, a third pressure-reducing device, at least one liquid nitrogen pump, and at least one gas-liquid separator.
[0019] Wherein, the high-pressure column and the low-pressure column are arranged substantially side-by-side, the first condenser evaporator is disposed at a bottom of the low-pressure column, and the second condenser evaporator is disposed at an upper part of the low-pressure column.
[0020] Further comprising a component for sending a processed feed air into the high-pressure column;
[0021] a component for sending at least a part of the high-pressure column bottom oxygen-rich stream to the low-pressure column after pressure reduction via the first pressure-reducing device;
[0022] a component for sending at least a part of the first condenser evaporator bottom liquid to the second condenser evaporator after pressure reduction via the second pressure-reducing device;
[0023] a component for feeding the low-pressure nitrogen-rich vapor from the top of the low-pressure column into the second condenser evaporator, and a component for sending the first portion of low-pressure liquid nitrogen obtained after condensation back to the top of the low-pressure column and a component for sending the second portion of low-pressure liquid nitrogen to an inlet of the liquid nitrogen pump;
[0024] a component for feeding the high-pressure nitrogen-rich vapor from the top of the high-pressure column into the first condenser evaporator, and a component for feeding the high-pressure liquid nitrogen obtained after condensation into the gas-liquid separator after pressure reduction via the third pressure-reducing device;
[0025] a component for sending a liquid phase from the gas-liquid separator to the inlet of the liquid nitrogen pump and a component for sending a gas phase from the gas-liquid separator to the top of the low-pressure column;
[0026] a component connecting an outlet of the liquid nitrogen pump to the top of the high-pressure column, and optionally further comprising a component for conveying a high-pressure nitrogen gas product produced at the top of the high-pressure column and / or the oxygen-rich waste gas stream produced at a top of the second condenser evaporator out of the distillation column system;
[0027] Additionally, further comprising a component for sending a flash gas generated at the outlet of the liquid nitrogen pump to the gas-liquid separator.
[0028] In another aspect, further comprising a subcooler, the subcooler comprising a cold-source passage and a hot-source passage, an inlet of the cold-source passage being connected to the outlet of the liquid nitrogen pump, an outlet thereof being connected to the top of the high-pressure column, an inlet of the hot-source passage being connected to an outlet of the high-pressure liquid nitrogen of the first condenser evaporator, and an outlet thereof being connected to an inlet of the third pressure-reducing device.
[0029] Further, the first condenser evaporator is immersed in the low-pressure column bottom oxygen-rich stream.
[0030] Preferably, the distillation column system of the present invention is suitable for a nitrogen generator.
[0031] Compared with a dual-column stacked arrangement, the dual-column side-by-side arrangement of the present invention can reduce the size of the columns and the cold box, facilitating transportation and installation.
[0032] The use of the subcooler reduces the amount of flashed gas and improves the nitrogen extraction rate.
[0033] By using the gas-liquid separator to recover the post-flash gas, the nitrogen extraction rate is further improved.
[0034] The design of arranging the first condenser evaporator at the bottom of the low-pressure column reduces the number of liquid pumps and saves investment costs.BRIEF DESCRIPTION OF THE DRAWINGS
[0035] The advantages and spirit of the present invention can be further understood through the following detailed description of the invention and the accompanying drawings.
[0036] FIG. 1 is a schematic flowchart of a dual-column side-by-side arrangement in Comparative Example 1;
[0037] FIG. 2 is a schematic flowchart of a dual-column side-by-side arrangement in Comparative Example 2;
[0038] FIG. 3 is a schematic flowchart of a dual-column side-by-side arrangement in Embodiment 1;
[0039] FIG. 4 is a schematic flowchart of a dual-column side-by-side arrangement in Embodiment 2;
[0040] In the figures, the same reference labels represent corresponding streams or components.
[0041] In the figures, the same reference numerals represent corresponding streams or components, wherein: 01-high-pressure column; 02-low-pressure column; 03-first condenser evaporator; 04-second condenser evaporator; 05-first pressure-reducing device; 06-second pressure-reducing device; 07-liquid nitrogen pump; 08-oxygen-rich stream pump; 09-gas-liquid separator; 10-third pressure-reducing device; 11-subcooler; 20-feed air; 21-high-pressure column bottom oxygen-rich stream; 22-high-pressure nitrogen-rich vapor; 23-high-pressure liquid nitrogen; 24-first condenser evaporator bottom liquid; 25-low-pressure nitrogen-rich vapor; 26-first portion of low-pressure liquid nitrogen; 27-second portion of low-pressure liquid nitrogen; 28-oxygen-rich waste gas stream; 29-low-pressure column bottom oxygen-rich stream; 30-high-pressure nitrogen gas product; 31-high-pressure column reflux liquid; 32-gas-liquid separator gas phase; 33-gas-liquid separator liquid phase; 34-flash gas.
[0042] DETAILED DESCRIPTION OF THE EMBODIMENTS
[0043] Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. However, it should be understood that the present invention is not limited to the embodiments described below, and the technical concept of the present invention can be implemented in combination with other known technologies or other technologies whose functions are the same as those known technologies.
[0044] The terms "first" and "second" are used for descriptive purposes only, and are not intended to limit the time sequence, quantity, or importance, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated, but merely to distinguish one technical feature from another in the present technical solution. Thus, a feature defined with "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, the meaning of "multiple" is two or more, unless otherwise explicitly and specifically stated. Similarly, a limiter appearing herein, such as "a" or "an" , is not intended to be a limitation of quantity, but rather describes a technical feature that has not appeared previously. Similarly, unless a noun is modified by a specific quantitative word, it shall be regarded herein as including both singular and plural forms, and in this technical solution, it may include a single one of the technical feature, or plural ones of the technical feature. Words such as "only" and "solely" should be understood as specific quantitative words, indicating that the noun they define is one and only one.
[0045] Modifiers such as "about" or "approximately" appearing before a numeral herein usually include the numeral itself, and their specific meaning should be understood in combination with the context. When a numeral appears as an endpoint of a numerical range, the numerical range includes the values of the two endpoints; similarly, when a numerical value appears as an endpoint of an open-ended range, for example, in connection with "at least" , "at most" , "not greater than" , "not less than" , "not higher than" , "not lower than" , the open-ended numerical range also includes the value of the endpoint.
[0046] It should be understood that, in the present invention, "at least one (time) " means one (time) or multiple (times) . "And / or" is used to describe the association relationship of associated objects, indicating that three relationships may exist, for example, "A and / or B" may represent: only A exists, only B exists, and both A and B exist, where A and B may be singular or plural.
[0047] As used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items. Unless otherwise specified, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It should also be understood that terms, such as those defined in commonly used dictionaries, should be understood as having a meaning that is consistent with their meaning in the context of this specification and the relevant art, and should not be interpreted in an idealized or overly formal sense unless expressly so defined herein. For the sake of brevity and / or clarity, well-known functions or constructions may not be described in detail.
[0048] Natural pressure losses are generally not included in pressure data. If the pressure difference between corresponding parts is not greater than the natural line loss caused by pressure loss in pipelines, heat exchangers, coolers, adsorbers, ordinary regulating valves (non-throttle valves) , etc., the pressure is rated as "equal" here. The "pressure" and "pressure range" in the present invention may accommodate a certain error, and the unit used is absolute pressure. For a specific set of cryogenic air separation equipment or a cryogenic air separation process, the pressure ranges do not overlap.
[0049] A "column" in the present invention refers to a pressure vessel having a substantially continuous shell (except for openings provided for pipelines, channels, or devices such as condenser evaporators) , wherein trays or packing provided in the shell allow a mixture to be separated therein by distillation. When the distillation column system of the present invention comprises at least two columns, the column with a relatively higher operating pressure is referred to as a high-pressure column, and the column with a relatively lower operating pressure is referred to as a low-pressure column. For reasons such as convenient transportation, installation, reducing footprint, or reducing the height of the distillation column, the high-pressure column and / or the low-pressure column may be split into several parts and assembled in a suitable manner.
[0050] "Distillation column system" refers to all columns involved in distillation and the pipelines, valves, condenser evaporators, and other devices connected to the columns. A "component" in the present invention comprises a pipeline, a passage, a valve, or other necessary equipment. Taking "a component for sending the high-pressure column bottom oxygen-rich stream to the low-pressure column after pressure reduction via the first pressure-reducing device" as an example, the component comprises a pipeline with one end connected to the high-pressure column bottom and one end connected to the low-pressure column, the first pressure-reducing device, optional valves, etc., so that the oxygen-rich stream can flow from the high-pressure column bottom into the low-pressure column along the component. Other components besides the distillation column system are omitted from the drawings of the present invention, but those skilled in the art will understand that a conventional cryogenic air separation apparatus also comprises a main air compressor, an air precooling and purification system, a main heat exchanger, a combination of an air compressor and an expander, other cooling capacity providing components, or subcoolers, etc. As needed, other components can be combined with the distillation column system in the present invention to achieve cryogenic air separation.
[0051] In the present invention, the high-pressure column and the low-pressure column are arranged substantially side-by-side, which arrangement is opposite to stacking the two. In a side-by-side arrangement, a lowest point of either column is not higher than a highest point of the other column. Preferably, both columns are arranged above the ground.
[0052] A "pressure-reducing device" in the present invention comprises any equipment that causes the fluid pressure at an outlet end to be lower than the fluid pressure at an inlet end. For example, the pressure-reducing device may be a pressure-reducing valve or an expander.
[0053] A "condenser evaporator" in a cryogenic air separation apparatus is a heat exchange device that condenses one stream (generally nitrogen-rich vapor from a column top) and evaporates another stream (generally an oxygen-rich liquid) through indirect heat exchange, so as to provide the reflux liquid or rising gas required for distillation. Indirect heat exchange can be achieved through a plate-fin heat exchange unit. Classified by liquid immersion method, condenser evaporators include two types: falling film and bath-type. In the present invention, a bath-type condenser evaporator is preferred.
[0054] The criteria for "above" and "below" in the present invention are the absolute distance relative to the installation ground. Taking a distillation column comprising a high-pressure column and / or a low-pressure column as an example, the part where distillation trays or packing are provided is the rectifying section of the column. A component, for example a condenser evaporator, being "above" a high-pressure column or a low-pressure column means that the relative distance of the component from the ground is higher than a top of the rectifying section of the column; a component, for example a condenser evaporator, being "below" a high-pressure column or a low-pressure column means that the relative distance of the component from the ground is lower than a bottom of the rectifying section of the column; however, "above" or "below" does not limit the relative relationship between the component and the shell of the distillation column. For example, a condenser evaporator located above the low-pressure column can be placed either inside the shell of the low-pressure column or outside the shell of the low-pressure column.
[0055] The "top" and "bottom" of a column in the present invention are also relative to the rectifying section of the column. The part above the rectifying section in a column is the top of the column, and the part below the rectifying section is the bottom of the column.
[0056] FIG. 1 discloses a situation as Comparative Example 1 where a high-pressure column 01 and a low-pressure column 02 are arranged substantially side-by-side. In FIG. 1, there are two condenser evaporators in total, namely a first condenser evaporator 03 located above the high-pressure column 01 and a second condenser evaporator 04 located above the low-pressure column 02. Both condenser evaporators may be, for example, bath-type. An operating pressure of the high-pressure column 01 may be, for example, about 10 bara, and an operating pressure of the low-pressure column 02 may be, for example, about 4.5 bara. A feed air 20, after being pressurized, precooled, purified, and refrigerated by a main heat exchanger (not shown in FIG. 1) , has a temperature between -130℃ and -170℃, and is free of impurities such as H2O, CO2, and other hydrocarbons. This feed air 20 is fed to a lower part of the high-pressure column 01, and after rectification therein, a high-pressure column bottom oxygen-rich stream 21 is obtained at a bottom, and a high-pressure nitrogen-rich vapor 22 is generated at a top. The high-pressure column bottom oxygen-rich stream 21 is reduced in pressure and introduced into the first condenser evaporator 03 to indirectly heat exchange with the high-pressure nitrogen-rich vapor 22 entering it. The high-pressure nitrogen-rich vapor 22 is condensed to obtain a high-pressure liquid nitrogen 23, and the high-pressure column bottom oxygen-rich stream 21 is partially evaporated to generate a first condenser evaporator bottom liquid 24, and the first condenser evaporator bottom liquid 24 is sent to the low-pressure column 02 for distillation. The first condenser evaporator bottom liquid 24 is further rectified in the low-pressure column 02 to obtain a low-pressure column bottom oxygen-rich stream 29 at a bottom and to generate a low-pressure nitrogen-rich vapor 25 at a top. In the second condenser evaporator 04, the pressure-reduced low-pressure column bottom oxygen-rich stream 29 indirectly heat exchanges with the low-pressure nitrogen-rich vapor 25 from the top of the low-pressure column 02. The former is partially evaporated to obtain an oxygen-rich waste gas stream 28, which is discharged from a top of the second condenser evaporator 04, and the latter is condensed to obtain a low-pressure liquid nitrogen. A first portion of low-pressure liquid nitrogen 26 returns to the top of the low-pressure column 02, and a second portion of low-pressure liquid nitrogen 27 is pressurized by a liquid nitrogen pump 07 and sent back to the top of the high-pressure column 01, together with the high-pressure liquid nitrogen 23, as a reflux liquid for the high-pressure column. This distillation column system can produce a large amount of high-pressure nitrogen gas product 30.
[0057] FIG. 2 discloses a situation as Comparative Example 2 where a high-pressure column 01 and a low-pressure column 02 are arranged substantially side-by-side. An operating pressure of the high-pressure column 01 may be, for example, about 10 bara, and an operating pressure of the low-pressure column 02 may be, for example, about 4.5 bara. A feed air 20, after being pressurized, precooled, purified, and refrigerated by a main heat exchanger (not shown in FIG. 2) , has a temperature between -130℃ and -170℃, and is free of impurities such as H2O, CO2, and other hydrocarbons. This feed air 20 is fed to a lower part of the high-pressure column 01, and after rectification therein, a high-pressure column bottom oxygen-rich stream 21 is obtained at a bottom, and a high-pressure nitrogen-rich vapor 22 is generated at a top. The high-pressure column bottom oxygen-rich stream 21 passes through a first pressure-reducing device 05 and is introduced into the low-pressure column 02, and after further rectification therein, a low-pressure column bottom oxygen-rich stream 29 is obtained at a bottom, and a low-pressure nitrogen-rich vapor 25 is generated at a top. In FIG. 2, there are two condenser evaporators in total, namely a first condenser evaporator 03 located above the high-pressure column 01 and a second condenser evaporator 04 located above the low-pressure column 02. Both condenser evaporators may be, for example, bath-type. The first condenser evaporator 03 receives the low-pressure column bottom oxygen-rich stream 29 from the bottom of the low-pressure column 02, and this stream indirectly heat exchanges with the high-pressure nitrogen-rich vapor 22 from the top of the high-pressure column 01. The former is partially evaporated to generate a first condenser evaporator bottom liquid 24, and the latter is condensed to obtain a high-pressure liquid nitrogen 23. The first condenser evaporator bottom liquid 24 is reduced in pressure via a second pressure-reducing device 06 and introduced into the second condenser evaporator 04, and this stream indirectly heat exchanges with the low-pressure nitrogen-rich vapor 25 from the top of the low-pressure column 02. The former is partially evaporated to obtain an oxygen-rich waste gas stream 28, which is discharged from a top of the second condenser evaporator 04, and the latter is condensed to obtain a low-pressure liquid nitrogen. A first portion of low-pressure liquid nitrogen 26 returns to the top of the low-pressure column 02 as a reflux liquid, and a second portion of low-pressure liquid nitrogen 27 is pressurized by a liquid nitrogen pump 07 and sent back to the top of the high-pressure column 01, together with the high-pressure liquid nitrogen 23, as a reflux liquid for the high-pressure column. This distillation column system can produce a large amount of high-pressure nitrogen gas product. In this process, the pressure in the first condenser evaporator 03 is approximately equal to the operating pressure of the low-pressure column 02. Since the two columns are arranged side-by-side, the low-pressure column bottom oxygen-rich stream 29 cannot flow into the first condenser evaporator 03 under the action of gravity, and this stream must be pumped into the first condenser evaporator 03 by an oxygen-rich stream pump 08.
[0058] In Comparative Example 1, since the high-pressure column bottom oxygen-rich stream 21 directly enters the first condenser evaporator 03 without utilizing the rectifying section of the low-pressure column 02, the nitrogen extraction rate is not optimized. In Comparative Example 2, two liquid pumps are used, resulting in high equipment investment. Meanwhile, the liquid stream is prone to flashing at the outlet of the pump, which reduces the nitrogen extraction rate. The two embodiments in FIG. 3 and FIG. 4 overcome the above disadvantages.
[0059] In Embodiment 1 disclosed in FIG. 3, by adjusting the relative positions of various parts, the entire distillation column system includes only one pump.
[0060] The high-pressure column 01 and the low-pressure column 02 are arranged substantially side-by-side. The difference from Comparative Example 2 is that the first condenser evaporator 03 is arranged below the rectifying section of the low-pressure column 02, and preferably, the first condenser evaporator 03 is arranged at the bottom of the low-pressure column 02, so as to be directly immersed in the low-pressure column bottom oxygen-rich stream 29. The second condenser evaporator 04 is still arranged above the low-pressure column 02. Specifically, an operating pressure of the high-pressure column may be, for example, about 10 bara, and an operating pressure of the low-pressure column may be, for example, about 4.5 bara.
[0061] A feed air 20, after being pressurized, precooled, purified, and refrigerated by a main heat exchanger (not shown in FIG. 3) , has a temperature between -130℃ and -170℃, and is free of impurities such as H2O, CO2, and other hydrocarbons. A pipeline for this feed air 20 is connected to a lower part of the high-pressure column 01.
[0062] The feed air 20 is rectified in the high-pressure column 01 to obtain a high-pressure column bottom oxygen-rich stream 21 at a bottom and to generate a high-pressure nitrogen-rich vapor 22 at a top. The high-pressure column bottom oxygen-rich stream 21 is reduced in pressure via a first pressure-reducing device 05 and introduced into the low-pressure column 02, and after further rectification therein, a low-pressure column bottom oxygen-rich stream 29 is obtained at a bottom, and a low-pressure nitrogen-rich vapor 25 is generated at a top.
[0063] The first condenser evaporator 03 receives the low-pressure column bottom oxygen-rich stream 29 from the bottom of the low-pressure column 02, and this stream indirectly heat exchanges with the high-pressure nitrogen-rich vapor 22 from the top of the high-pressure column 01. The former is partially evaporated to generate a first condenser evaporator bottom liquid 24, and the latter is condensed to obtain a high-pressure liquid nitrogen 23. The pressure of the high-pressure liquid nitrogen 23 is approximately equal to the operating pressure of the high-pressure column, i.e., about 10 bara. The first condenser evaporator bottom liquid 24 is reduced in pressure via a second pressure-reducing device 06 and introduced into the second condenser evaporator 04, and this stream indirectly heat exchanges with the low-pressure nitrogen-rich vapor 25 from the top of the low-pressure column 02.
[0064] The first condenser evaporator bottom liquid 24 is partially evaporated to obtain an oxygen-rich waste gas stream 28. The oxygen-rich waste gas stream 28 is discharged from a top of the second condenser evaporator 04, and the low-pressure nitrogen-rich vapor 25 is condensed to obtain a low-pressure liquid nitrogen.
[0065] A first portion of low-pressure liquid nitrogen 26 returns to the top of the low-pressure column 02 as a reflux liquid. The pressure of the low-pressure liquid nitrogen is approximately equal to the operating pressure of the low-pressure column, i.e., about 4.5 bara.
[0066] Embodiment 1 is provided with a gas-liquid separator 09, and the pressure in the gas-liquid separator 09 is approximately equal to the operating pressure of the low-pressure column 02. The high-pressure liquid nitrogen 23 passes through a third pressure-reducing device 10, and its pressure drops to approximately the operating pressure of the low-pressure column 02. Due to the pressure drop, part of the liquid in the stream flashes into gas at this time, and in the gas-liquid separator 09, the stream is separated into a liquid phase and a gas phase.
[0067] A gas-liquid separator liquid phase 33 merges with a second portion of low-pressure liquid nitrogen 27 from the second condenser evaporator 04. The merged stream is pressurized by a liquid nitrogen pump 07 to obtain a high-pressure column liquid nitrogen reflux liquid 31, which returns to the top of the high-pressure column 01 as a reflux liquid for the high-pressure column. At an outlet of the liquid nitrogen pump 07, nitrogen gas may be generated due to flashing. This part of the gas can preferably be sent back to the gas-liquid separator 09, and merged therein with the gas-phase product from the high-pressure liquid nitrogen 23, to obtain a gas-liquid separator gas phase 32. This stream 32 returns to the low-pressure column 02.
[0068] Compared with Comparative Example 1, the nitrogen extraction rate is increased by about 2%, and a large amount of high-pressure nitrogen gas product 30 can be produced. Compared with Comparative Example 2, since the low-pressure column bottom oxygen-rich stream 29 can directly enter the first condenser evaporator 03 for heat exchange, no additional oxygen-rich stream pump is needed, saving equipment expenditure. Meanwhile, the flow rate through the liquid nitrogen pump 07 in Embodiment 1 is approximately 3 times the liquid nitrogen flow rate in the two comparative examples, which allows for the selection of a centrifugal pump even for a nitrogen generator with a small air separation capacity. Compared with a piston pump, which is the only choice at low flow rates, a centrifugal pump has the advantages of low vibration and low maintenance.
[0069] The difference between Embodiment 2 disclosed in FIG. 4 and Embodiment 1 is mainly reflected in the addition of a subcooler 11, so that the high-pressure liquid nitrogen 23 is subcooled before entering the third pressure-reducing device 10. Specifically, the high-pressure column 01 and the low-pressure column 02 are arranged substantially side-by-side, the first condenser evaporator 03 is arranged below the rectifying section of the low-pressure column 02, and preferably, the first condenser evaporator 03 is arranged at the bottom of the low-pressure column 02, so as to be directly immersed in the low-pressure column bottom oxygen-rich stream 29. The second condenser evaporator 04 is still arranged above the low-pressure column 02. An operating pressure of the high-pressure column 01 may be, for example, about 10 bara, and an operating pressure of the low-pressure column 02 may be, for example, about 4.5 bara.
[0070] A feed air 20, after being pressurized, precooled, purified, and refrigerated by a main heat exchanger (not shown in FIG. 4) , has a temperature between -130℃ and -170℃, and is free of impurities such as H2O, CO2, and other hydrocarbons. A pipeline for this feed air 20 is connected to a lower part of the high-pressure column 01. The feed air 20 is rectified in the high-pressure column 01 to obtain a high-pressure column bottom oxygen-rich stream 21 at a bottom and to generate a high-pressure nitrogen-rich vapor 22 at a top.
[0071] The high-pressure column bottom oxygen-rich stream 21 is reduced in pressure via a first pressure-reducing device 05 and introduced into the low-pressure column 02, and after further rectification therein, a low-pressure column bottom oxygen-rich stream 29 is obtained at a bottom, and a low-pressure nitrogen-rich vapor 25 is generated at a top.
[0072] The first condenser evaporator 03 receives the low-pressure column bottom oxygen-rich stream 29 from the bottom of the low-pressure column 02, and this stream indirectly heat exchanges with the high-pressure nitrogen-rich vapor 22 from the top of the high-pressure column 01. The former is partially evaporated to generate a first condenser evaporator bottom liquid 24, and the latter is condensed to obtain a high-pressure liquid nitrogen 23. The pressure of the high-pressure liquid nitrogen 23 is approximately equal to the operating pressure of the high-pressure column, i.e., about 10 bara.
[0073] The first condenser evaporator bottom liquid 24 is reduced in pressure via a second pressure-reducing device 06 and introduced into the second condenser evaporator 04, and this stream indirectly heat exchanges with the low-pressure nitrogen-rich vapor 25 from the top of the low-pressure column 02. The first condenser evaporator bottom liquid 24 is partially evaporated to obtain an oxygen-rich waste gas stream 28, and the oxygen-rich waste gas stream 28 is discharged from a top of the second condenser evaporator 02; the low-pressure nitrogen-rich vapor 25 is condensed to obtain a low-pressure liquid nitrogen. A first portion of low-pressure liquid nitrogen 26 returns to the top of the low-pressure column as a reflux liquid. The pressure of the low-pressure liquid nitrogen is approximately equal to the operating pressure of the low-pressure column 02, i.e., about 4.5 bara.
[0074] Embodiment 2 is provided with a gas-liquid separator 09, and the pressure in the gas-liquid separator 09 is approximately equal to the operating pressure of the low-pressure column 02.
[0075] A subcooler 11 is also provided, the subcooler 11 having at least one hot-source passage and one cold-source passage. The hot-source passage refers to the passage through which a stream providing heat in the subcooler 11 flows; after providing heat, this stream is subcooled and its temperature decreases. The cold-source passage refers to the passage through which a stream receiving heat in the subcooler flows; after receiving heat, this stream's temperature increases.
[0076] An inlet of the cold-source passage of the subcooler 11 is connected to an outlet of the liquid nitrogen pump 07, and an outlet thereof is connected to the top of the high-pressure column 01. An inlet of the hot-source passage of the subcooler 11 is connected to an outlet of the high-pressure liquid nitrogen 23 of the first condenser evaporator 03, and an outlet thereof is connected to an inlet of the third pressure-reducing device 10.
[0077] The high-pressure liquid nitrogen 23 passes through the third pressure-reducing device 10, and its pressure drops to approximately the operating pressure of the low-pressure column 02.
[0078] Due to the pressure drop, part of the liquid in the stream flashes into gas at this time. The lower the temperature of the high-pressure liquid nitrogen 23, the smaller the amount of gas generated after flashing.
[0079] In the gas-liquid separator 09, the pressure-reduced high-pressure liquid nitrogen is separated into a liquid phase and a gas phase. A gas-liquid separator liquid phase 33 merges with a second portion of low-pressure liquid nitrogen 27 from the second condenser evaporator 04. The merged stream is pressurized by a liquid nitrogen pump 07 to obtain a high-pressure column liquid nitrogen reflux liquid 31, which returns to the top of the high-pressure column 01 as a reflux liquid for the high-pressure column.
[0080] At an outlet of the liquid nitrogen pump 07, nitrogen gas may be generated due to flashing. This part of the gas can preferably be sent back to the gas-liquid separator 09, and merged therein with the gas-phase product from the high-pressure liquid nitrogen 23, to obtain a gas-liquid separator gas phase 32, which returns to the low-pressure column 02.
[0081] In this embodiment, the pressurized high-pressure column liquid nitrogen reflux liquid 31 and the high-pressure liquid nitrogen 23 heat exchange in the subcooler 11. After heat exchange, the temperature of the high-pressure liquid nitrogen 23 is reduced, thereby reducing the amount of gas generated in the subsequent multiple flashing processes, thus improving the nitrogen extraction rate.
[0082] Compared with Embodiment 1, the nitrogen extraction rate in Embodiment 2 is increased by about 1%; compared with Comparative Example 1, the nitrogen extraction rate in Embodiment 2 is increased by a total of about 3%, and a large amount of high-pressure nitrogen gas product 30 can be produced.
[0083] The present invention is not only applicable to the above embodiments, but also applicable to any process flow using at least two distillation columns, including processes for producing nitrogen, or simultaneously producing multiple gases such as nitrogen, oxygen, and argon. What is described in this specification are only preferred specific embodiments of the present invention, and the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit the present invention. Any technical solution obtained by those skilled in the art based on the concept of the present invention through logical analysis, reasoning, or limited experimentation should fall within the scope of the present invention.
Claims
1.A method for cryogenically separating air, characterized by:providing a main air compressor, an air precooling and purification system, a main heat exchanger, and a distillation column system, the distillation column system comprising at least one high-pressure column and one low-pressure column, a first condenser evaporator and a second condenser evaporator, a first pressure-reducing device, a second pressure-reducing device, a third pressure-reducing device, at least one liquid nitrogen pump, and at least one gas-liquid separator;heat exchanging and liquefying a feed air that has been precooled and purified following compression by the main air compressor in the main heat exchanger against a return stream from the distillation column system, and then feeding the feed air into a lower part of the high-pressure column;rectifying the feed air in the high-pressure column to produce a high-pressure column bottom oxygen-rich stream at a bottom of the high-pressure column and to produce a high-pressure nitrogen-rich vapor at a top of the high-pressure column;reducing pressure of at least a part of the high-pressure column bottom oxygen-rich stream via the first pressure-reducing device, feeding the at least part of the high-pressure column bottom oxygen-rich stream into the low-pressure column arranged substantially side-by-side, and rectifying it in the low-pressure column to produce a low-pressure column bottom oxygen-rich stream at a bottom of the low-pressure column and to produce a low-pressure nitrogen-rich vapor at a top of the low-pressure column;the first condenser evaporator, disposed at the bottom of the low-pressure column, receiving the high-pressure nitrogen-rich vapor from the top of the high-pressure column and heat exchanging the high-pressure nitrogen-rich vapor with the low-pressure column bottom oxygen-rich stream, to condense the high-pressure nitrogen-rich vapor to obtain a high-pressure liquid nitrogen, and to partially evaporate the low-pressure column bottom oxygen-rich stream to generate a first condenser evaporator bottom liquid;the second condenser evaporator, disposed at an upper part of the low-pressure column, receiving the low-pressure nitrogen-rich vapor from the top of the low-pressure column and heat exchanging the low-pressure nitrogen-rich vapor with the first condenser evaporator bottom liquid that has been reduced in pressure via the second pressure-reducing device, to condense the low-pressure nitrogen-rich vapor to obtain a low-pressure liquid nitrogen, at least a first portion of the low-pressure liquid nitrogen serving as a low-pressure column reflux liquid, and to partially evaporate the first condenser evaporator bottom liquid to generate an oxygen-rich waste gas stream and discharge the oxygen-rich waste gas stream;reducing pressure of at least a part of the high-pressure liquid nitrogen via the third pressure-reducing device and feeding the at least part of the high-pressure liquid nitrogen into the gas-liquid separator, wherein a gas phase separated therein is sent back to an upper part of the low-pressure column, and a liquid phase separated therein is pressurized by the liquid nitrogen pump and then fed into the high-pressure column as a high-pressure column reflux liquid;the low-pressure liquid nitrogen further comprises a second portion of low-pressure liquid nitrogen, the second portion of low-pressure liquid nitrogen merging with the liquid phase from the gas-liquid separator, being pressurized by the liquid nitrogen pump, and then fed into the high-pressure column as the high-pressure column reflux liquid.2.The method of claim 1, characterized by sending a flash gas generated downstream of the liquid nitrogen pump back to the gas-liquid separator.3.The method of claim 2, characterized by further comprising a subcooler, wherein the high-pressure column reflux liquid, before returning to the high-pressure column, indirectly heat exchanges with the high-pressure liquid nitrogen in the subcooler, and the subcooled high-pressure liquid nitrogen is reduced in pressure via the third pressure-reducing device and then fed into the gas-liquid separator.4.A distillation column system suitable for the method for cryogenically separating air of claim 1, characterized by comprising at least one high-pressure column and one low-pressure column, a first condenser evaporator and a second condenser evaporator, a first pressure-reducing device, a second pressure-reducing device, a third pressure-reducing device, at least one liquid nitrogen pump, and at least one gas-liquid separator, wherein the high-pressure column and the low-pressure column are arranged substantially side-by-side, the first condenser evaporator is disposed at a bottom of the low-pressure column, and the second condenser evaporator is disposed at an upper part of the low-pressure column;further comprising a component for sending a processed feed air into the high-pressure column;a component for sending at least a part of the high-pressure column bottom oxygen-rich stream to the low-pressure column after pressure reduction via the first pressure-reducing device,a component for sending at least a part of the first condenser evaporator bottom liquid to the second condenser evaporator after pressure reduction via the second pressure-reducing device,a component for feeding the low-pressure nitrogen-rich vapor from the top of the low-pressure column into the second condenser evaporator,and a component for sending the first portion of low-pressure liquid nitrogen obtained after condensation back to the top of the low-pressure column and a component for sending the second portion of low-pressure liquid nitrogen to an inlet of the liquid nitrogen pump,a component for feeding the high-pressure nitrogen-rich vapor from the top of the high-pressure column into the first condenser evaporator,and a component for feeding the high-pressure liquid nitrogen obtained after condensation into the gas-liquid separator after pressure reduction via the third pressure-reducing device,a component for sending a liquid phase from the gas-liquid separator to the inlet of the liquid nitrogen pump and a component for sending a gas phase from the gas-liquid separator to the top of the low-pressure column,a component connecting an outlet of the liquid nitrogen pump to the top of the high-pressure column, and optionally further comprising a component for conveying a high-pressure nitrogen gas product produced at the top of the high-pressure column and / or the oxygen-rich waste gas stream produced at a top of the second condenser evaporator out of the distillation column system.5.The distillation column system of claim 4, characterized by further comprising a component for sending a flash gas generated at the outlet of the liquid nitrogen pump to the gas-liquid separator.6.The distillation column system of claim 4 or 5, characterized by further comprising a subcooler, the subcooler comprising a cold-source passage and a hot-source passage, an inlet of the cold-source passage being connected to the outlet of the liquid nitrogen pump, an outlet of the cold-source passage being connected to the top of the high-pressure column, an inlet of the hot-source passage being connected to an outlet of the high-pressure liquid nitrogen of the first condenser evaporator, and an outlet of the hot-source passage being connected to an inlet of the third pressure-reducing device.7.The distillation column system of claim 4, characterized in that the first condenser evaporator is immersed in the low-pressure column bottom oxygen-rich stream.8.The distillation column system of claim 4, characterized in that the distillation column system is suitable for a nitrogen generator.