EP1760415A1 - Verfahren und Vorrichtung zur Gewinnung von Argon durch Tieftemperaturzerlegung von Luft - Google Patents

Verfahren und Vorrichtung zur Gewinnung von Argon durch Tieftemperaturzerlegung von Luft Download PDF

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Publication number
EP1760415A1
EP1760415A1 EP05425609A EP05425609A EP1760415A1 EP 1760415 A1 EP1760415 A1 EP 1760415A1 EP 05425609 A EP05425609 A EP 05425609A EP 05425609 A EP05425609 A EP 05425609A EP 1760415 A1 EP1760415 A1 EP 1760415A1
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EP
European Patent Office
Prior art keywords
column
argon
fed
heat exchanger
crude
Prior art date
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Application number
EP05425609A
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English (en)
French (fr)
Inventor
Emanuele Bigi
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SIAD MACCHINE IMPIANTI SpA
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SIAD MACCHINE IMPIANTI SpA
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Publication date
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Priority to EP05425609A priority Critical patent/EP1760415A1/de
Publication of EP1760415A1 publication Critical patent/EP1760415A1/de
Withdrawn legal-status Critical Current

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
    • F25J3/04727—Producing pure argon, e.g. recovered from a crude argon column using an auxiliary pure argon column for nitrogen rejection
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04969—Retrofitting or revamping of an existing air fractionation unit
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/58—Processes or apparatus involving steps for recycling of process streams the recycled stream being argon or crude argon

Definitions

  • the present invention relates to an argon production plant and the relative process, and more particularly to a plant for argon production by low temperature fractionation of air, and the relative process.
  • Cryogenic rectification is a known system for separating argon from other atmospheric gases.
  • the air is compressed, purified, cooled and fed to a conventional air rectification column preferably divided into two sections.
  • the main air separation products, oxygen and nitrogen, can be obtained directly from the rectification column at the required purity level.
  • the boiling point (87.8 K at 1 bar) of which lies between the boiling point of oxygen (90.2 K at 1 bar) and nitrogen (77.4 K at 1 bar) is consequently enriched within the central region of the upper column section. A fraction with maximum argon enrichment is withdrawn from this region.
  • the argon-rich fraction is fed to a crude argon column, where oxygen is partially removed. Consequently, the product has still to be purified of the remaining oxygen and nitrogen at the exit of the crude argon column.
  • the oxygen can be removed only partially in the crude argon column, because the boiling points of argon and oxygen are extremely close together. The difference in their boiling points is 2.9 K at a pressure of 1 bar.
  • the remainder of the oxygen is normally removed by a deoxo unit in which the product is mixed with hydrogen, the oxygen then being burnt with the formation of water.
  • a deoxo unit is a costly apparatus with high running costs because of its considerable hydrogen consumption.
  • An object of the present invention is to provide an argon production plant and relative process, which is of lower installation and operating cost than those of the known art.
  • Another object is to enable already existing plants to be easily and economically converted to obtain plants of equal or superior performance with lower running and maintenance costs.
  • a process for producing argon by low temperature air fractionation comprising the following steps: feeding a rectification column of at least one section with said air; extracting from said rectification column an argon-containing fraction and feeding it to a crude argon column; extracting from said crude argon column an argon-containing fraction and feeding it to a nitrogen removal column; and extracting from said nitrogen removal column an argon-containing fraction and feeding it to a pure argon column.
  • a plant for producing argon by low temperature air fractionation comprising a rectification column of at least one section fed with said air; a crude argon column fed with an argon-containing fraction withdrawn from said rectification column; a nitrogen removal column fed with an argon-containing fraction withdrawn from said crude argon column; and a pure argon column fed with an argon-containing fraction withdrawn from said nitrogen removal column.
  • the argon production plant consists of a conventional rectification column with two portions or sections, comprising a high pressure column 12 and a low pressure column 14.
  • the air comprising mainly oxygen, nitrogen and argon, is fed into the column 12 through the pipe 10.
  • the column 12 has between 30 and 50 theoretical stages, the column 14 having between 50 and 90 theoretical stages.
  • a fraction of the product is withdrawn from a suitable region of the column 14 (between stage 20 and stage 40) where the argon concentration is a maximum and the nitrogen concentration is low, and is fed to the bottom of a crude argon column 16 via a pipe 18.
  • a condenser heat exchanger 20 is present, fed via the pipe 21 with oxygen-rich liquid, i.e. with about 30-45% of oxygen (O 2 ), about 55-70% of nitrogen (N 2 ) and about 1-2% of argon (Ar), originating from the pipe 42, or with crude liquid argon originating from the bottom of the column 32.
  • oxygen-rich liquid i.e. with about 30-45% of oxygen (O 2 ), about 55-70% of nitrogen (N 2 ) and about 1-2% of argon (Ar)
  • the condenser heat exchanger 20 discharges vapour at the same composition as that entering through the pipe 42, and returns it either to the column 14 in a region between the exits of the pipes 18 and 40 at a point where the oxygen-rich mixture has an equal or similar oxygen (O 2 ) percentage, or to the column 32 if in the form of crude argon in the gaseous state.
  • the argon withdrawn from the crude argon column 16 via the pipe 22 has a concentration between 96 and 99.9%, and is fed to an intermediate point of a nitrogen removal column 24.
  • the nitrogen removal column 24 has between 30 and 60 theoretical stages.
  • a condenser heat exchanger 26 is present, fed with liquid nitrogen via the pipe 29, at a pressure between 1.1 and 2 bar, which enables the argon and oxygen fraction present in the column 24 to condense. whereas the nitrogen fraction (0.1-4%) which does not condense (because the nitrogen condensation temperature is lower than the condenser temperature), is discharged to atmosphere through the pipe 50.
  • the liquid nitrogen fed to the condenser heat exchanger 26 through the pipe 29, vaporizes and is discharged via the pipe 25 and fed to the main heat exchanger (not shown, the purpose of which is to cool the air entering through the pipe 10).
  • a reboiler heat exchanger 28 is present, fed via the pipe 27 with gaseous nitrogen at a pressure between 3 and 7 bar and a temperature close to its liquefaction temperature.
  • This nitrogen is liquefied by the argon mixture fraction present on the other side of the reboiler heat exchanger 28, and is fed to the condenser heat exchanger 26 via the pipe 29.
  • Argon collects in the bottom of the column 24 with a nitrogen content less than 10 ppm and with a residual oxygen percentage corresponding to the feed fraction, and hence preferably between 10 ppm and 5%, as it depends on the number of stages present in the crude argon column 16. Typically the number of theoretical stages of the crude argon column 16 is between 40 and 145.
  • this percentage is normally between 1% and 2% (with about 40 theoretical stages).
  • the argon withdrawn from the column 24 is fed via the pipe 30 to a pure argon column 32.
  • the number of theoretical stages of the pure argon column 32 is between 40 and 120 and depends on the residual oxygen fraction present in the feed; the lower the oxygen fraction, the smaller the number of theoretical stages required.
  • a reflux condenser 36 is present in the top of the pure argon column 32, the bottom of which contains a reboiler heat exchanger 36.
  • the condenser heat exchanger 34 is fed either with a liquid argon fraction withdrawn from the column 14 at low pressure and hence via the pipe 40, or with a liquid argon fraction withdrawn from the column 12 at high pressure and hence via the pipe 41, or with an oxygen-rich liquid fraction withdrawn from the column 12 at high pressure and hence via the pipe 42, or with fluid withdrawn from the reboiler heat exchanger 36 via the pipe 44.
  • the condenser heat exchanger 34 discharges through the pipe 35, either into the main plant heat exchanger if in the form of nitrogen in the gaseous state, or into the column 14 in a region between the exits of the pipes 18 and 40 at a point where the oxygen-rich mixture has an equal or similar oxygen (O 2 ) percentage.
  • the reboiler heat exchanger 36 is fed either with compressed air or with compressed nitrogen, or with crude argon vapour leaving the top of the crude argon column 16, in which case it becomes the reboiler heat exchanger for the pure argon column 32 and the condenser for the crude argon column 16.
  • Argon which is practically oxygen-free (less than 10 ppm) and nitrogen-free (as this was eliminated in the previous column) can be withdrawn from the top of the pure argon column 32 through the pipe 48.
  • the oxygen-rich liquid stream 52 is withdrawn from the bottom of the column 32 and fed to the lower part of the crude argon column 16.
  • the columns 12, 14, 16, 24 and 32 can comprise either plates or structured fillings or random fillings, either individually or combined.
  • Such plants are normally formed from a two-section rectification column followed by a deoxo unit and a nitrogen removal column in succession.
  • the deoxo unit is removed, and the connection which connected the two-section rectification column to the deoxo unit is now made directly to the nitrogen removal column.
  • a pure argon column is installed and positioned in series after the nitrogen removal column. A plant in accordance with the present invention is obtained in this manner.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
EP05425609A 2005-08-31 2005-08-31 Verfahren und Vorrichtung zur Gewinnung von Argon durch Tieftemperaturzerlegung von Luft Withdrawn EP1760415A1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP05425609A EP1760415A1 (de) 2005-08-31 2005-08-31 Verfahren und Vorrichtung zur Gewinnung von Argon durch Tieftemperaturzerlegung von Luft

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP05425609A EP1760415A1 (de) 2005-08-31 2005-08-31 Verfahren und Vorrichtung zur Gewinnung von Argon durch Tieftemperaturzerlegung von Luft

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EP1760415A1 true EP1760415A1 (de) 2007-03-07

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014169989A1 (de) * 2013-04-18 2014-10-23 Linde Aktiengesellschaft Nachrüstbare vorrichtung zur tieftemperaturzerlegung von luft, nachrüstanlage und verfahren zum nachrüsten einer tieftemperatur-luftzerlegungsanlage
CN113739515A (zh) * 2021-09-06 2021-12-03 乔治洛德方法研究和开发液化空气有限公司 一种通过富氩气提取高纯液氩的方法和装置

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE821951C (de) * 1949-06-20 1951-11-22 Linde Eismasch Ag Verfahren zur Gewinnung von Argon
JPH0777385A (ja) * 1993-06-30 1995-03-20 Nippon Sanso Kk 高純度アルゴンの分離方法及びその装置
JPH07127971A (ja) * 1993-11-02 1995-05-19 Nippon Sanso Kk アルゴンの分離装置
DE19743731A1 (de) * 1996-10-02 1998-04-09 Linde Ag Verfahren und Vorrichtung zur Gewinnung von reinem Argon
US5970743A (en) * 1998-06-10 1999-10-26 Air Products And Chemicals, Inc. Production of argon from a cryogenic air separation process

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE821951C (de) * 1949-06-20 1951-11-22 Linde Eismasch Ag Verfahren zur Gewinnung von Argon
JPH0777385A (ja) * 1993-06-30 1995-03-20 Nippon Sanso Kk 高純度アルゴンの分離方法及びその装置
JPH07127971A (ja) * 1993-11-02 1995-05-19 Nippon Sanso Kk アルゴンの分離装置
DE19743731A1 (de) * 1996-10-02 1998-04-09 Linde Ag Verfahren und Vorrichtung zur Gewinnung von reinem Argon
US5970743A (en) * 1998-06-10 1999-10-26 Air Products And Chemicals, Inc. Production of argon from a cryogenic air separation process

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 1995, no. 06 31 July 1995 (1995-07-31) *
PATENT ABSTRACTS OF JAPAN vol. 1995, no. 08 29 September 1995 (1995-09-29) *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014169989A1 (de) * 2013-04-18 2014-10-23 Linde Aktiengesellschaft Nachrüstbare vorrichtung zur tieftemperaturzerlegung von luft, nachrüstanlage und verfahren zum nachrüsten einer tieftemperatur-luftzerlegungsanlage
CN113739515A (zh) * 2021-09-06 2021-12-03 乔治洛德方法研究和开发液化空气有限公司 一种通过富氩气提取高纯液氩的方法和装置
CN113739515B (zh) * 2021-09-06 2022-10-21 乔治洛德方法研究和开发液化空气有限公司 一种通过富氩气提取高纯液氩的方法和装置

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