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WO2009087324A2 - Column for separating a carbon monoxide and nitrogen mixture by cryogenic distillation, and apparatus including such column - Google Patents

Column for separating a carbon monoxide and nitrogen mixture by cryogenic distillation, and apparatus including such column Download PDF

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Publication number
WO2009087324A2
WO2009087324A2 PCT/FR2008/052290 FR2008052290W WO2009087324A2 WO 2009087324 A2 WO2009087324 A2 WO 2009087324A2 FR 2008052290 W FR2008052290 W FR 2008052290W WO 2009087324 A2 WO2009087324 A2 WO 2009087324A2
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WO
WIPO (PCT)
Prior art keywords
column
nitrogen
carbon monoxide
mixture
methane
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/FR2008/052290
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French (fr)
Other versions
WO2009087324A3 (en
Inventor
Marc Wagner
Natacha Haik-Beraud
Daniel Machon Diez De Baldeon
Jean-Jacques Talbot
Antoine Hernandez
Philippe Grigoletto
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Filing date
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Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of WO2009087324A2 publication Critical patent/WO2009087324A2/en
Anticipated expiration legal-status Critical
Publication of WO2009087324A3 publication Critical patent/WO2009087324A3/en
Ceased legal-status Critical Current

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Classifications

    • 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
    • F25J3/0228—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 characterised by the separated product stream
    • F25J3/028—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 characterised by the separated product stream separation of noble gases
    • F25J3/0285—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 characterised by the separated product stream separation of noble gases of argon
    • 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
    • F25J3/0204—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 characterised by the feed stream
    • F25J3/0219—Refinery gas, cracking gas, coke oven gas, gaseous mixtures containing aliphatic unsaturated CnHm or gaseous mixtures of undefined nature
    • 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
    • F25J3/0228—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 characterised by the separated product stream
    • F25J3/0252—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 characterised by the separated product stream separation of hydrogen
    • 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
    • F25J3/0228—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 characterised by the separated product stream
    • F25J3/0257—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 characterised by the separated product stream separation of nitrogen
    • 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
    • F25J3/0228—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 characterised by the separated product stream
    • F25J3/0261—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 characterised by the separated product stream separation of carbon monoxide
    • 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
    • F25J3/04763—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
    • F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
    • F25J3/04884—Arrangement of reboiler-condensers
    • 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
    • F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • F25J5/002—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger
    • F25J5/005—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger in a reboiler-condenser, e.g. within a 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
    • 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
    • F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead gas
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/20—H2/N2 mixture, i.e. synthesis gas for or purge gas from ammonia synthesis
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/04—Down-flowing type boiler-condenser, i.e. with evaporation of a falling liquid film
    • 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
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/40—Vertical layout or arrangement of cold equipments within in the cold box, e.g. columns, condensers, heat exchangers etc.

Definitions

  • the present invention relates to a separation column of a mixture of carbon monoxide and nitrogen or a mixture of carbon monoxide and methane or a mixture of nitrogen and argon and optionally methane by cryogenic distillation and to an apparatus incorporating such a column.
  • Apparatus for separating mixtures of carbon monoxide and hydrogen more and more often include a column for purifying carbon monoxide to nitrogen.
  • This separation column includes an overhead vaporizer-condenser to be included within a capacity.
  • thermosiphon vaporizer immersed in a bath of liquid carbon monoxide.
  • thermosiphon vaporizer-condenser has the following drawbacks:
  • the capacity of the vaporizer-condenser has a larger section than the CO-N2 column, which contributes to increase unnecessarily the section of the envelope of the cold box
  • thermosiphon vaporizer • We seek a relatively high exchange performance, which leads to a high volume of exchanger due to the limitations of the thermosiphon vaporizer.
  • Plate and finned film vaporizers are known for air separation in the "Developments in Falling Film Type (Downflow) Reboilers in the Air Separation Industry" by Chakravarty et al., Fifth International Conferenc on Enhanced, Compact and Ultra Compact Heat Exchangers, Hoboken, September 2005 and Trace Component Accumulation in Downflow Reboilers by Houghton et al, 2000 AIChE Spring Meeting, Atlanta, March 2000.
  • a film vaporizer as the head condenser of a carbon monoxide and nitrogen separation column or a carbon monoxide and methane separation column.
  • the film vaporizer is inclined with respect to the vertical with an inclination angle ranging from 1 ° to 10 °;
  • the mixture has as main components carbon monoxide and nitrogen;
  • the mixture has as main components carbon monoxide and methane;
  • the vaporizer is constituted by a plate and finned exchanger.
  • an apparatus for separation by cryogenic distillation of a mixture having, as main components, carbon monoxide, hydrogen, nitrogen and possibly methane comprising at least one column. as described above.
  • the liquid is vaporized at least 98% or 100% at the output of the film vaporizer.
  • the process of separation by cryogenic distillation preferably separates a mixture having as main components carbon monoxide, hydrogen, nitrogen and possibly methane.
  • FIG. 1 represents a part of an apparatus for separating a mixture of carbon monoxide, hydrogen, methane and nitrogen and whose figures 2, 2a and 3 show a film evaporator with plates and fins adapted for use in a column according to the invention.
  • a mixture 1 of carbon monoxide and methane is sent to column K3 to be separated into a methane-rich tank liquid 21 and a carbon monoxide-rich overhead gas 23.
  • the top condenser V1 of the column K3 is a condenser according to FR-A-2916523 with a heat exchanger 5 surrounded by a barrier.
  • the condenser V1 may be of the plate and finned film vaporizer type.
  • the sum of the liquids grouped in the fluid 3 coming from a cycle is sent to the condenser V1 where it vaporises to form a gas 25.
  • Part of the tank liquid 4 of the condenser V1 is sent to a vaporizer V2 of the line of main exchange, for example a thermosiphon of the main exchange line.
  • V5 is the sub-cooler of the methane washing column, V5 being able to work as a thermosiphon on the subcooler of the methane wash column and the remainder of the liquid 9 is sent to the head condenser V9 of a nitrogen and carbon monoxide separation column K4 fed by at least a portion of the gas 23 from the head of the column K3.
  • a nitrogen-rich gas is withdrawn at the outlet of the exchanger 25 and a carbon monoxide-rich liquid 13 is withdrawn in the tank and sent to the top condenser V9.
  • the heat exchanger 25 is fed with the liquids 9, 13 and serves to condense the nitrogen at the top of the column K4.
  • the exchanger 25 functions as a film vaporizer.
  • Part of the liquid 17 of the condenser V9 is sent to the vaporizer V2 of the main exchange line (V2 may be a thermosiphon of the main exchange line).
  • the 5.25 film vaporizer has a low section configuration and high volume thermal performance.
  • the amount of liquid CO in the capacity of the vaporizer is minimal because it is reduced to the excess liquid at the outlet of the vaporizer.
  • the conventional film vaporizer has a defect in this application in that it is normally designed not to vaporize the entire liquid, because for the exchange is good, it is necessary that the liquid to vaporize remains two-phase on all the path of the vaporization. This poses a reduced running problem in the case of a column CO / N 2 , such as K4. Indeed, the liquid to be vaporized consists for the most part of the bottom liquid of the tank of the column CO / N 2 , which is then reassembled in the vaporizer V9 due to the pressure difference between the column and the capacity vaporizer.
  • the film vaporizer is designed not to vaporize all the liquid in normal operation, with a reduced run, we will vaporize all the liquid and at the same time condense more CO / N vapor 2 from the top of the column, which will lead to a drop in pressure and instabilities due to a hydraulic piston defect to raise the liquid CO from the bottom of the column vessel to the vaporizer.
  • the exchanger is supplied with liquid through a pipe 9 which sends liquid through a valve 33 and the pipe 35 directly above the open passages of the film vaporizer 25.
  • Figure 2bis shows a film vaporizer at the top of the separation column CO / CH4 K3 where another pipe 39 connected to the pipe 3 by a valve 37 directly feeds the liquid bath around the exchanger 5, the outlet of the steam 23 being at the top of column CO / CH 4 K3.
  • the vaporizer is inclined at 5 ° from vertical V but the inclination can vary between 1 ° and 10 ° vertically.
  • the invention is also applicable to ammonia synthesis purge gas treatment processes and apparatus using columns which separate mixtures having nitrogen and argon as main components and / or mixtures having as their main components main components of nitrogen, argon and methane.
  • the separation column used may have a head condenser comprising a plate and finned film vaporizer.
  • the liquid vaporizing in the condenser may be carbon monoxide, nitrogen or other liquid.

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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)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention relates to a cryogenic distillation separation column (K4) for separating a mixture including, as main components, carbon monoxide and either methane or nitrogen, wherein said column includes a head condenser (V9) comprising a film vaporiser (25).

Description

Colonne de séparation d'un mélange de monoxyde de carbone et d'azote par distillation cryogénique et appareil incorporant une telle colonne Column for separating a mixture of carbon monoxide and nitrogen by cryogenic distillation and apparatus incorporating such a column

La présente invention est relative à une colonne de séparation d'un mélange de monoxyde de carbone et d'azote ou d'un mélange de monoxyde de carbone et de méthane ou d'un mélange d'azote et d'argon et éventuellement de méthane par distillation cryogénique et à un appareil incorporant une telle colonne.The present invention relates to a separation column of a mixture of carbon monoxide and nitrogen or a mixture of carbon monoxide and methane or a mixture of nitrogen and argon and optionally methane by cryogenic distillation and to an apparatus incorporating such a column.

Les appareils de séparation des mélanges de monoxyde de carbone et d'hydrogène comprennent de plus en plus souvent une colonne permettant d'épurer le monoxyde de carbone en azote.Apparatus for separating mixtures of carbon monoxide and hydrogen more and more often include a column for purifying carbon monoxide to nitrogen.

Cette colonne de séparation comprend un vaporiseur-condenseur en tête à inclure à l'intérieur d'une capacité.This separation column includes an overhead vaporizer-condenser to be included within a capacity.

Les références de la société demanderesse jusqu'ici étaient basées sur un vaporiseur en thermosiphon immergé dans un bain de monoxyde de carbone liquide.The references of the applicant company so far were based on a thermosiphon vaporizer immersed in a bath of liquid carbon monoxide.

Un vaporiseur-condenseur en thermosiphon présente les inconvénients suivants :A thermosiphon vaporizer-condenser has the following drawbacks:

• Une quantité importante de liquide contenue dans la capacité du vaporiseur, ce qui contribue largement à l'encours global en monoxyde de carbone de la boite froide, pose un problème de sécurité et conduit à un surdimensionnement des traitements des purges cryogéniques.• A large quantity of liquid contained in the vaporizer's capacity, which largely contributes to the overall amount of carbon monoxide in the cold box, poses a safety problem and leads to over-sizing the cryogenic purge treatments.

• La capacité du vaporiseur-condenseur a une section plus importante que la colonne CO-N2, ce qui contribue à augmenter inutilement la section de l'enveloppe de la boite froide• The capacity of the vaporizer-condenser has a larger section than the CO-N2 column, which contributes to increase unnecessarily the section of the envelope of the cold box

• On cherche une performance en échange relativement élevée, ce qui conduit à un volume d'échangeur élevé du fait des limitations des vaporiseur en thermosiphon.• We seek a relatively high exchange performance, which leads to a high volume of exchanger due to the limitations of the thermosiphon vaporizer.

Les vaporiseurs à film à plaques et à ailettes sont connus pour la séparation d'air dans les documents « Developments in Falling Film Type (Downflow) Reboilers in the Air Séparation Industry » de Chakravarty et al., Fifth International Conferenc on Enhanced, Compact and Ultra Compact Heat Exchangers, Hoboken, septembre 2005 et « Trace Component Accumulation in Downflow Reboilers » de Houghton et al, 2000 AIChE Spring Meeting, Atlanta, mars 2000.Plate and finned film vaporizers are known for air separation in the "Developments in Falling Film Type (Downflow) Reboilers in the Air Separation Industry" by Chakravarty et al., Fifth International Conferenc on Enhanced, Compact and Ultra Compact Heat Exchangers, Hoboken, September 2005 and Trace Component Accumulation in Downflow Reboilers by Houghton et al, 2000 AIChE Spring Meeting, Atlanta, March 2000.

Selon la présente invention, il est prévu d'utiliser un vaporiseur à film comme condenseur de tête d'une colonne de séparation de monoxyde de carbone et d'azote ou d'une colonne de séparation de monoxyde de carbone et de méthane.According to the present invention, it is intended to use a film vaporizer as the head condenser of a carbon monoxide and nitrogen separation column or a carbon monoxide and methane separation column.

Selon un aspect de l'invention, il est prévu une colonne de séparation par distillation cryogénique d'un mélange ayant comme composants principaux i) du monoxyde de carbone et soit du méthane soit de l'azote ou ii) de l'azote, de l'argon et éventuellement du méthane, la colonne ayant un condenseur de tête caractérisée en ce que le condenseur de tête est constitué par un vaporiseur à film.According to one aspect of the invention, there is provided a cryogenic distillation separation column of a mixture having as main components i) carbon monoxide and either methane or nitrogen or ii) nitrogen, argon and optionally methane, the column having a head condenser characterized in that the head condenser is constituted by a film evaporator.

Selon d'autres aspects facultatifs :According to other optional aspects:

- le vaporiseur à film est incliné par rapport à la verticale avec un angle d'inclinaison allant de 1 ° à 10° ;the film vaporizer is inclined with respect to the vertical with an inclination angle ranging from 1 ° to 10 °;

- le mélange a comme composants principaux du monoxyde de carbone et de l'azote ;the mixture has as main components carbon monoxide and nitrogen;

- le mélange a comme composants principaux du monoxyde de carbone et du méthane ; le vaporiseur est constitué par un échangeur à plaques et à ailettes.the mixture has as main components carbon monoxide and methane; the vaporizer is constituted by a plate and finned exchanger.

Selon un autre aspect de l'invention, il est prévu un appareil de séparation par distillation cryogénique d'un mélange ayant comme composants principaux du monoxyde de carbone, de l'hydrogène, de l'azote et éventuellement du méthane comprenant au moins une colonne comme décrite ci-dessus. Selon un autre objet de l'invention, il est prévu un procédé de séparation par distillation cryogénique d'un mélange ayant comme composants principaux du monoxyde de carbone et soit du méthane soit de l'azote utilisant une colonne telle que décrite ci-dessus.According to another aspect of the invention, there is provided an apparatus for separation by cryogenic distillation of a mixture having, as main components, carbon monoxide, hydrogen, nitrogen and possibly methane comprising at least one column. as described above. According to another object of the invention, there is provided a method of separation by cryogenic distillation of a mixture having as main components of carbon monoxide and either methane or nitrogen using a column as described above.

Optionnellement :Optionally:

- au moins dans une marche le liquide est vaporisé à au moins 98%, voire 100% en sortie du vaporiseur à film.- At least in one step the liquid is vaporized at least 98% or 100% at the output of the film vaporizer.

Le procédé de séparation par distillation cryogénique sépare de préférence un mélange ayant comme composants principaux du monoxyde de carbone, de l'hydrogène, d'azote et éventuellement du méthane.The process of separation by cryogenic distillation preferably separates a mixture having as main components carbon monoxide, hydrogen, nitrogen and possibly methane.

L'invention sera décrite en plus de détail par rapport aux figures, dont la figure 1 représente une partie d'un appareil de séparation d'un mélange de monoxyde de carbone, d'hydrogène, de méthane et d'azote et dont les figures 2, 2 bis et 3 représentent un vaporiseur à film à plaques et à ailettes adapté à être utilisé dans une colonne selon l'invention. Dans la Figure 1 , un mélange 1 de monoxyde de carbone et de méthane est envoyé à la colonne K3 pour être séparé en un liquide de cuve 21 riche en méthane et un gaz de tête 23 riche en monoxyde de carbone.The invention will be described in more detail with respect to the figures, of which FIG. 1 represents a part of an apparatus for separating a mixture of carbon monoxide, hydrogen, methane and nitrogen and whose figures 2, 2a and 3 show a film evaporator with plates and fins adapted for use in a column according to the invention. In Figure 1, a mixture 1 of carbon monoxide and methane is sent to column K3 to be separated into a methane-rich tank liquid 21 and a carbon monoxide-rich overhead gas 23.

Le condenseur de tête V1 de la colonne K3 est un condenseur selon FR- A-2916523 avec un échangeur 5 entouré d'une barrière. Le condenseur V1 peut être du type vaporiseur à film à plaques et à ailettes. La somme des liquides regroupés dans le fluide 3 provenant d'un cycle est envoyée au condenseur V1 où il se vaporise pour former un gaz 25. Une partie du liquide de cuve 4 du condenseur V1 est envoyée à un vaporiseur V2 de la ligne d'échange principale, par exemple un thermosiphon de la ligne d'échange principale. Une autre partie 7 du liquide peut être envoyée à un vaporiseur V5 Dans le cas d'un procédé lavage au méthane , V5 est le sous- refroidisseur de la colonne de lavage au méthane, V5 pouvant fonctionner en thermosiphon sur le sous-refroidisseur de la colonne de lavage au méthane et le reste du liquide 9 est envoyé au condenseur de tête V9 d'une colonne de séparation d'azote et de monoxyde de carbone K4 alimentée par une partie au moins du gaz 23 provenant de la tête de la colonne K3. Un gaz riche en azote 15 est prélevé en sortie de l'échangeur 25 et un liquide 13 riche en monoxyde de carbone est soutiré en cuve et envoyé au condenseur de tête V9. L'échangeur de chaleur 25 est alimenté par les liquides 9,13 et sert à condenser l'azote de tête de la colonne K4. L'échangeur 25 fonctionne comme un vaporiseur à film. Une partie du liquide 17 du condenseur V9 est envoyée au vaporiseur V2 de la ligne d'échange principale (V2 pouvant être un thermosiphon de la ligne d'échange principale).The top condenser V1 of the column K3 is a condenser according to FR-A-2916523 with a heat exchanger 5 surrounded by a barrier. The condenser V1 may be of the plate and finned film vaporizer type. The sum of the liquids grouped in the fluid 3 coming from a cycle is sent to the condenser V1 where it vaporises to form a gas 25. Part of the tank liquid 4 of the condenser V1 is sent to a vaporizer V2 of the line of main exchange, for example a thermosiphon of the main exchange line. Another part 7 of the liquid can be sent to a vaporizer V5 In the case of a methane washing process, V5 is the sub-cooler of the methane washing column, V5 being able to work as a thermosiphon on the subcooler of the methane wash column and the remainder of the liquid 9 is sent to the head condenser V9 of a nitrogen and carbon monoxide separation column K4 fed by at least a portion of the gas 23 from the head of the column K3. A nitrogen-rich gas is withdrawn at the outlet of the exchanger 25 and a carbon monoxide-rich liquid 13 is withdrawn in the tank and sent to the top condenser V9. The heat exchanger 25 is fed with the liquids 9, 13 and serves to condense the nitrogen at the top of the column K4. The exchanger 25 functions as a film vaporizer. Part of the liquid 17 of the condenser V9 is sent to the vaporizer V2 of the main exchange line (V2 may be a thermosiphon of the main exchange line).

Le vaporiseur à film 5,25 présente une configuration à faible section et à performance thermique au volume élevée.The 5.25 film vaporizer has a low section configuration and high volume thermal performance.

La quantité de CO liquide dans la capacité du vaporiseur est minimale car elle est réduite à l'excédent liquide en sortie du vaporiseur. • Le vaporiseur à film classique a toutefois un défaut dans cette application dans la mesure où il est normalement conçu pour ne pas vaporiser en totalité le liquide, car pour que l'échange soit bon, il faut que le liquide à vaporiser reste diphasique sur tout le trajet de la vaporisation. Ceci pose un problème à marche réduite dans le cas d'une colonne CO / N2, tel que K4. En effet, le liquide à vaporiser est constitué en majeure partie du liquide du fond de la cuve de la colonne CO / N2, lequel est ensuite remonté dans le vaporiseur V9 par le fait de l'écart de pression entre la colonne et la capacité du vaporiseur. Si le vaporiseur à film est conçu pour ne pas vaporiser tout le liquide en marche normale, à marche réduite on va vaporiser tout le liquide et en même temps condenser plus de vapeur CO / N2 du haut de la colonne, ce qui va conduire à une chute de la pression et à des instabilités du fait d'un défaut de piston hydraulique pour remonter le CO liquide du fond de cuve de colonne jusqu'au vaporiseur.The amount of liquid CO in the capacity of the vaporizer is minimal because it is reduced to the excess liquid at the outlet of the vaporizer. The conventional film vaporizer, however, has a defect in this application in that it is normally designed not to vaporize the entire liquid, because for the exchange is good, it is necessary that the liquid to vaporize remains two-phase on all the path of the vaporization. This poses a reduced running problem in the case of a column CO / N 2 , such as K4. Indeed, the liquid to be vaporized consists for the most part of the bottom liquid of the tank of the column CO / N 2 , which is then reassembled in the vaporizer V9 due to the pressure difference between the column and the capacity vaporizer. If the film vaporizer is designed not to vaporize all the liquid in normal operation, with a reduced run, we will vaporize all the liquid and at the same time condense more CO / N vapor 2 from the top of the column, which will lead to a drop in pressure and instabilities due to a hydraulic piston defect to raise the liquid CO from the bottom of the column vessel to the vaporizer.

La solution est de concevoir un vaporiseur à film dont le liquide est presque totalement vaporisé en sortie du vaporiseur dans les conditions de marche normale .Donc en cas de marche réduite, une partie importante du vaporiseur fonctionne en échange gaz/gaz, ce qui n'est pas du tout performant et va conduire à une augmentation de l'écart des températures. Dans les passages de condensation, de même les vapeurs ne seront pas totalement condensées ce qui entraîne une augmentation de la perte de charge et un envahissement liquide du bas du vaporiseur donc une réduction d'autant de sa performance. Dans la Figure 2, on voit l'échangeur à plaques et à ailettes 25 alimenté en azote gazeux par la conduite 29 reliant l'échangeur avec la tête de la colonne K4. L'azote liquide est renvoyé à la colonne par la conduite 31. Un débit d'azote 15 est soutiré généralement en sortie de l'échangeur 25. L'échangeur est alimenté en liquide par une conduite 9 qui envoie du liquide à travers une vanne 33 et la conduite 35 directement au-dessus des passages ouverts du vaporiseur à film 25. La Figure 2bis représente un vaporiseur à film en tête de colonne de séparation CO/CH4 K3 où une autre conduite 39 reliée à la conduite 3 par une vanne 37 permet d'alimenter directement le bain de liquide autour de l'échangeur 5, la sortie de la vapeur 23 se faisant en tête de colonne CO/CH4 K3.The solution is to design a film vaporizer whose liquid is almost completely vaporized at the outlet of the vaporizer under normal operating conditions. So in case of reduced running, a large part of the vaporizer operates in gas / gas exchange, which does not is not at all efficient and will lead to an increase in the difference in temperatures. In the condensation passages, the vapors will not be completely condensed resulting in an increase in the pressure drop and liquid invasion of the bottom of the vaporizer therefore a reduction of as much its performance. In Figure 2, the plate and fin exchanger 25 fed with nitrogen gas is seen through line 29 connecting the exchanger with the head of column K4. The liquid nitrogen is returned to the column by the pipe 31. A nitrogen flow 15 is withdrawn generally at the outlet of the exchanger 25. The exchanger is supplied with liquid through a pipe 9 which sends liquid through a valve 33 and the pipe 35 directly above the open passages of the film vaporizer 25. Figure 2bis shows a film vaporizer at the top of the separation column CO / CH4 K3 where another pipe 39 connected to the pipe 3 by a valve 37 directly feeds the liquid bath around the exchanger 5, the outlet of the steam 23 being at the top of column CO / CH 4 K3.

Une amélioration supplémentaire serait d'installer le vaporiseur à film 5,25 avec un angle faible par rapport à la verticale de manière à avoir une gamelle d'alimentation inclinée donc de dégager le liquide des passages extrêmes à bas niveau, ce qui réduit encore d'autant la surface effective d'échange à bas régime.An additional improvement would be to install the 5.25 film vaporizer at a small angle to the vertical so as to have a sloped feed bowl and thus to free the liquid from the low end passages, further reducing the effective exchange surface at low speed.

Ceci a certes pour effet de réduire les capacités d'échange du vaporiseur à marche partielle, contrairement à ce qui est habituellement recherché, et permet de sécher les canaux.This certainly has the effect of reducing the exchange capacity of the partial-walk vaporizer, contrary to what is usually sought, and allows the channels to dry.

Dans l'exemple le vaporiseur est incliné à 5° de la verticale V mais l'inclinaison peut varier entre 1 ° et 10° à la verticale.In the example, the vaporizer is inclined at 5 ° from vertical V but the inclination can vary between 1 ° and 10 ° vertically.

L'invention s'applique également aux procédés et aux appareils de traitement de gaz de purge de synthèse d'ammoniac utilisant des colonnes qui séparent des mélanges ayant pour composants principaux de l'azote et de l'argon et/ou des mélanges ayant pour composants principaux de l'azote, de l'argon et du méthane. Dans ces cas, la colonne de séparation utilisée peut avoir un condenseur de tête comprenant un vaporiseur à film à plaques et à ailettes. Le liquide se vaporisant dans le condenseur peut être du monoxyde de carbone, de l'azote ou un autre liquide. Des procédés de ce genre sont décrits dans « Séparation of Gases » d'Isalski, 1989, chapitre 6. The invention is also applicable to ammonia synthesis purge gas treatment processes and apparatus using columns which separate mixtures having nitrogen and argon as main components and / or mixtures having as their main components main components of nitrogen, argon and methane. In these cases, the separation column used may have a head condenser comprising a plate and finned film vaporizer. The liquid vaporizing in the condenser may be carbon monoxide, nitrogen or other liquid. Such methods are described in Isalski's Separation of Gases, 1989, Chapter 6.

Claims

REVENDICATIONS 1. Colonne de séparation (K3,K4) par distillation cryogénique d'un mélange (1 ,23) ayant comme composants principaux i) du monoxyde de carbone et soit du méthane soit de l'azote ou ii) de l'azote, de l'argon et éventuellement du méthane, la colonne ayant un condenseur de tête (5,25) caractérisée en ce que le condenseur de tête est constitué par un vaporiseur à film.1. Separation column (K3, K4) by cryogenic distillation of a mixture (1, 23) having as main components i) carbon monoxide and either methane or nitrogen or ii) nitrogen, argon and optionally methane, the column having a top condenser (5.25) characterized in that the top condenser is constituted by a film evaporator. 2. Colonne selon la revendication 1 dans lequel le vaporiseur à film2. Column according to claim 1 wherein the film vaporizer (5,25) est incliné par rapport à la verticale avec un angle d'inclinaison allant de 1 ° à 10°.(5.25) is inclined to the vertical with an inclination angle of 1 ° to 10 °. 3. Colonne selon la revendication 1 ou 2 de séparation d'un mélange (23) ayant comme composants principaux du monoxyde de carbone et de l'azote.3. Column according to claim 1 or 2 for separation of a mixture (23) having as main components carbon monoxide and nitrogen. 4. Colonne selon la revendication 1 ou 2 de séparation d'un mélange (1 ) ayant comme composants principaux du monoxyde de carbone et du méthane.4. Column according to claim 1 or 2 for separation of a mixture (1) having as main components carbon monoxide and methane. 5. Colonne selon la revendication 1 ou 2 de séparation d'un mélange ayant comme composants principaux de l'azote et de l'argon.5. Column according to claim 1 or 2 for separating a mixture having as main components nitrogen and argon. 6. Colonne selon la revendication 5 dans laquelle les composants principaux comprennent du méthane.The column of claim 5 wherein the main components comprise methane. 7. Colonne selon l'une des revendications précédentes dans lequel le vaporiseur à film est constitué par un échangeur à plaques et à ailettes.7. Column according to one of the preceding claims wherein the film vaporizer is constituted by a plate heat exchanger and fins. 8. Appareil de séparation par distillation cryogénique d'un mélange ayant comme composants principaux du monoxyde de carbone, de l'hydrogène, de l'azote et éventuellement du méthane comprenant au moins une colonne (K3, K4) selon l'une des revendications précédentes.8. Apparatus for the cryogenic distillation separation of a mixture having as main components carbon monoxide, hydrogen, nitrogen and optionally methane comprising at least one column (K3, K4) according to one of the preceding claims. 9. Procédé de séparation par distillation cryogénique d'un mélange (1 ,23) ayant comme composants principaux du monoxyde de carbone et soit du méthane soit de l'azote utilisant une colonne (K3,K4) selon l'une des revendications 1 à 4 ou 7 quand dépendante d'une des revendications 1 à 4.9. Process for the separation by cryogenic distillation of a mixture (1, 23) having as main components carbon monoxide and either methane or nitrogen using a column (K3, K4) according to one of claims 1 to 4 or 7 when dependent on one of claims 1 to 4. 10. Procédé selon la revendication 9 dans lequel au moins dans une marche le liquide (3,9,13) est vaporisé à au moins 98% , voire 100% en sortie du vaporiseur à film (5,25).10. The method of claim 9 wherein at least in one step the liquid (3,9,13) is vaporized at least 98%, or even 100% at the output of the film vaporizer (5.25). 11. Procédé de séparation par distillation cryogénique d'un mélange (1 ) ayant comme composants principaux du monoxyde de carbone, de l'hydrogène, d'azote et éventuellement du méthane comprenant une étape de procédé selon la revendication 9 ou 11.11. A method of separation by cryogenic distillation of a mixture (1) having as main components carbon monoxide, hydrogen, nitrogen and optionally methane comprising a process step according to claim 9 or 11. 12. Procédé de séparation par distillation cryogénique d'un mélange ayant comme composants principaux de l'azote et de l'argon en utilisant une colonne selon l'une des revendication 5, 6 ou 7 quand dépendante d'une des revendications 5 et 6.12. A method of separation by cryogenic distillation of a mixture having as main components of nitrogen and argon using a column according to one of claims 5, 6 or 7 when dependent on one of claims 5 and 6. . 13. Procédé selon la revendication 12 de séparation d'un mélange ayant comme composants principaux de l'azote, de l'argon et du méthane en utilisant une colonne selon la revendication 6 ou 7 quand dépendante de la revendication 6. 13. The method of claim 12 for separating a mixture having as major components nitrogen, argon and methane using a column according to claim 6 or 7 when dependent on claim 6.
PCT/FR2008/052290 2008-01-10 2008-12-12 Column for separating a carbon monoxide and nitrogen mixture by cryogenic distillation, and apparatus including such column Ceased WO2009087324A2 (en)

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US20130298600A1 (en) * 2011-01-17 2013-11-14 L'air Liquide Societe Anonyme Pour I'etude Et I'exploitation Des Procedes Georges Claude Process and apparatus for production of ammonia synthesis gas and pure methane by cryogenic separation

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US3992168A (en) * 1968-05-20 1976-11-16 Kobe Steel Ltd. Heat exchanger with rectification effect
DE3215829A1 (en) * 1982-04-28 1983-11-03 Linde Ag, 6200 Wiesbaden METHOD FOR PRODUCING CARBON MONOXIDE
WO1997001068A1 (en) * 1995-06-20 1997-01-09 Nippon Sanso Corporation Method and apparatus for separating argon
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US20130298600A1 (en) * 2011-01-17 2013-11-14 L'air Liquide Societe Anonyme Pour I'etude Et I'exploitation Des Procedes Georges Claude Process and apparatus for production of ammonia synthesis gas and pure methane by cryogenic separation

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