FR2636543A1 - Process and plant for treating a purge gas from an ammonium synthesis plant - Google Patents

Process and plant for treating a purge gas from an ammonium synthesis plant Download PDF

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Publication number
FR2636543A1
FR2636543A1 FR8811880A FR8811880A FR2636543A1 FR 2636543 A1 FR2636543 A1 FR 2636543A1 FR 8811880 A FR8811880 A FR 8811880A FR 8811880 A FR8811880 A FR 8811880A FR 2636543 A1 FR2636543 A1 FR 2636543A1
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Prior art keywords
nitrogen
hydrogen
ammonia
installation
argon
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FR2636543B1 (en
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Air Liquide SA
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Air Liquide SA
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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
    • F25J3/0228—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
    • F25J3/0276—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 H2/N2 mixtures, i.e. of ammonia synthesis gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/229—Integrated processes (Diffusion and at least one other process, e.g. adsorption, absorption)
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B23/00—Noble gases; Compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/04—Preparation of ammonia by synthesis in the gas phase
    • C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
    • C01C1/0476—Purge gas treatment, e.g. for removal of inert gases or recovery of H2
    • 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
    • F25J3/0233—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 CnHm with 1 carbon atom or more
    • 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
    • F25J3/028—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
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F25J2205/04—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/40—Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • F25J2205/66—Regenerating the adsorption vessel, e.g. kind of reactivation 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/80—Processes or apparatus using other separation and/or other processing means using membrane, i.e. including a permeation step
    • 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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/04—Recovery of liquid products
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/42—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being 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
    • F25J2240/00—Processes or apparatus involving steps for expanding of process streams
    • F25J2240/02—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream
    • 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
    • F25J2240/00—Processes or apparatus involving steps for expanding of process streams
    • F25J2240/02—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream
    • F25J2240/12—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream the fluid being 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/04—Internal refrigeration with work-producing gas expansion loop
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

The purge gas is purified from ammonia and water in 1 and 3 and partially condensed in 4 and the condensate is then distilled in 9 to separate the nitrogen, methane and argon. Hydrogen is separated off by means of a permeater 2 upstream of the heat exchanger 4 used for the partial condensation.

Description

DESCRIPTION
La présente invention est relative la séparation des constituants des gaz de purge des installations de synthèse d'ammoniac.DESCRIPTION
The present invention relates to the separation of the constituents of the purge gases from ammonia synthesis installations.

Ces gaz de purge contiennent, outre de l'ammoniac, de l'azote et de l'hydrogène, d'autres constituants (méthane, argon) qui peuvent être valorisés et qui ne sont pas réutilisables dans l'installation de synthèse d'ammoniac.  These purge gases contain, in addition to ammonia, nitrogen and hydrogen, other constituents (methane, argon) which can be recovered and which cannot be reused in the ammonia synthesis installation. .

Une technique classique pour effectuer cette séparation comprend un traitement primaire pour éliminer l'essentiel de l'ammoniac, une épuration par adsorption pour éliminer le reste de l'ammoniac et l'eau, une condensation partielle pour séparer l'hydrogène, et une distillation du condensat pour séparer l'azote, l'argon et le méthane, l'hydrogène et l'azote ainsi séparés étant recyclés au compresseur de l'installation de synthèse d' ammoniac. Cette technique permet certes de produire l'argon sous forme liquide, mais elle est coûteuse, car la partie cryogénique du procédé doit traiter un gaz non condensable (hydrogène) présent en proportion majoritaire voisine de 75 %. A conventional technique for effecting this separation includes a primary treatment to remove most of the ammonia, an adsorption treatment to remove the rest of the ammonia and water, partial condensation to separate the hydrogen, and distillation condensate to separate nitrogen, argon and methane, the hydrogen and nitrogen thus separated being recycled to the compressor of the ammonia synthesis installation. This technique certainly makes it possible to produce argon in liquid form, but it is expensive, because the cryogenic part of the process must treat a non-condensable gas (hydrogen) present in a majority proportion close to 75%.

L'invention a pour but de permettre d'obtenir les mêmes produits de façon plus économique du point de vue de l'investissement et/ou du coOt d'exploitation. The object of the invention is to make it possible to obtain the same products more economically from the point of view of investment and / or operating cost.

A cet effet, l'invention a pour objet un procédé du type précité, caractérisé en ce qu'il comprend une étape de séparation d'hydrogène par perméation en amont de l'étape de condensation. To this end, the subject of the invention is a method of the aforementioned type, characterized in that it comprises a step of hydrogen separation by permeation upstream of the condensation step.

Suivant un mode de mise en oeuvre avantageux, on liquéfie l'azote issu de la distillation, et l'on refroidit le mélange traité par vaporisation de l'azote liquide ainsi obtenu auquel on a ajouté une partie au moins du perméat de l'étape de perméation et/ou la vapeur issue de l'étape de condensation partielle. According to an advantageous embodiment, the nitrogen from the distillation is liquefied, and the treated mixture is cooled by vaporization of the liquid nitrogen thus obtained to which at least part of the permeate from step has been added. permeation and / or vapor from the partial condensation step.

L'invention a également pour objet une installation destinée a la mise en oeuvre d'un tel procédé. Cette installation, du type comprenant un appareil de traitement primaire destiné a éliminer l'essentiel de l'ammoniac, un appareil d'épuration par adsorption destiné å éliminer le reste de l'ammoniac et l'eau, un échangeur de chaleur indirect destiné a condenser l'ensemble des constituants restants sauf l'hydrogène, un appareil de distillation du condensat destin a séparer l'azote, l'argon et le méthane, et des moyens pour recycler l'azote et l'hydrogène au compresseur de l'installation de synthèse d'ammoniac, est caractérisée en ce qu'elle comprend un permeateur en#amont de l'échangeur de chaleur. The invention also relates to an installation intended for the implementation of such a method. This installation, of the type comprising a primary treatment device intended to remove the main part of the ammonia, an adsorption purification device intended to remove the rest of the ammonia and the water, an indirect heat exchanger intended to condensing all of the remaining constituents except hydrogen, a condensate distillation apparatus intended to separate nitrogen, argon and methane, and means for recycling nitrogen and hydrogen to the compressor of the installation of ammonia synthesis, is characterized in that it comprises a permeator upstream of the heat exchanger.

Quelques exemples de mise en oeuvre de l'invention vont maintenant être décrits en regard des dessins annexés, sur lesquels - la figure 1 représente schématiquement une installation suivant l'invention ; - les figures 2 et 3 représentent schématiquement deux variantes de la partie Il de la figure 1 ; et - les figures 4 et 5 représentent schématiquement deux autres variantes de l'installation de la figure 1. Some examples of implementation of the invention will now be described with reference to the accompanying drawings, in which - Figure 1 schematically shows an installation according to the invention; - Figures 2 and 3 schematically represent two variants of part II of Figure 1; and - Figures 4 and 5 schematically represent two other variants of the installation of Figure 1.

L'installation représentée la figure l est destinée a séparer les constituants du gaz de purge d'une installation de synthèse d'ammoniac. Ce gaz contient quelques * d'argon, de méthane et d'ammoniac, le reste étant partage entre l'hydrogène et l'azote dans des proportions d'environ 3/4-1/4. The installation shown in FIG. 1 is intended to separate the constituents of the purge gas from an ammonia synthesis installation. This gas contains a few * of argon, methane and ammonia, the rest being divided between hydrogen and nitrogen in proportions of approximately 3/4-1 / 4.

Le but de la séparation est de recycler l'azote et l'hydrogène au compresseur (non représenté) de l'installation de synthèse et de produire d'une part de l'argon liquide, d'autre part un gaz résiduaire constitué essentiellement de méthane et pouvant être valorisé en tant que "fuel gas". The purpose of the separation is to recycle the nitrogen and hydrogen to the compressor (not shown) of the synthesis installation and to produce on the one hand liquid argon, on the other hand a waste gas consisting essentially of methane and can be used as "fuel gas".

L'installation comprend essentiellement un appareil 1- de traitement primaire ; un perméateur 2 ; un appareil 3 d'épuration par adsorption ; un échangeur de chaleur indirect 4 a circulation contre-courant des fluides mis en relation d'échange thermique, équipé d'un séparateur de phases 5 a son bout froid, d'un compresseur de cycle 6, d'une turbine de détente 7 et d'une pompe froide 8 ; et un appareil 9 de distillation du condensat recueilli dans le séparateur 5, constitué par deux colonnes de distillation 10 et 11. The installation essentially comprises a primary treatment apparatus 1-; a permeator 2; an adsorption purification device 3; an indirect heat exchanger 4 with counter-current circulation of the fluids placed in heat exchange relationship, equipped with a phase separator 5 at its cold end, a cycle compressor 6, an expansion turbine 7 and a cold pump 8; and an apparatus 9 for distilling the condensate collected in the separator 5, constituted by two distillation columns 10 and 11.

L'appareil 1 est une colonne de lavage a l'eau alimentée en tete par de l'eau et a sa base par le gaz a traiter. Cette colonne produit en cuve un mélange liquide eau-ammoniac et délivre en tète le gaz partiellement épuré. The apparatus 1 is a water washing column supplied at the head with water and at its base with the gas to be treated. This column produces in the tank a liquid water-ammonia mixture and delivers at the head the partially purified gas.

Le perméateur 2 est adapté pour séparer l'hydrogène des autres constituants du mélange qui y est introduit, par exemple grâce a un faisceau de fibres creuses constituées par une membrane a perméabilité sélective. Un exemple de membrane convenant pour cette application est base sur une technologie polyaramide développée par DU PONT de NEMOURS selon le brevet Re 30351 (reissue de US. 3 899 309). D'autres exemples sont décrits dans les brevets US. 4 180 553 et US. 4 230 463. The permeator 2 is adapted to separate the hydrogen from the other constituents of the mixture which is introduced therein, for example by means of a bundle of hollow fibers formed by a membrane with selective permeability. An example of a membrane suitable for this application is based on a polyaramid technology developed by DU PONT de NEMOURS according to patent Re 30351 (reissue from US 3,899,309). Other examples are described in the US patents. 4,180,553 and US. 4,230,463.

L'appareil 3 comprend deux bouteilles d'adsorption 12 & BR< fonctionnement alterné, l'une étant en phase d'adsorption pendant que l'autre est en phase de régénération ou désorption a contre-courant. The apparatus 3 comprises two adsorption bottles 12 & BR <alternating operation, one being in the adsorption phase while the other is in the regeneration or counter-current desorption phase.

L'adsorbant contenu dans les bouteilles 12 est par exemple du tamis moléculaire. Cet appareil 3 est alimenté par une conduite 13 véhiculant le mélange a traiter, et par une conduite 14 véhiculant le gaz de régénération. Il comprend un ensemble de vannes approprié pour le fonctionnement qui sera décrit plus loin.The adsorbent contained in the bottles 12 is, for example, a molecular sieve. This device 3 is supplied by a pipe 13 conveying the mixture to be treated, and by a pipe 14 conveying the regeneration gas. It includes a set of valves suitable for operation which will be described later.

On décrira maintenant le fonctionnement de l'installation. Les valeurs numériques indiquées ne le sont qu' titre d'exemple et constituent seulesient des ordres de grandeur. The operation of the installation will now be described. The numerical values indicated are only an example and constitute only orders of magnitude.

Le gaz à traiter arrive a la colonne de lavage 1 puis dans le perméateur 2 a la pression de la boucle de synthèse d'ammoniac, soit 100 a 250 bars. Il est débarrassé d'une grande partie de l'ammoniac qu'il contient dans l'appareil 1, et d'une grande partie de l'hydrogène qu'il contient dans le perméateur 2, lequel produit sous une pression moyenne de 70 a 80 bars un perméat constitué essentiellement d'hydrogène et recyclé vers l'installation de synthèse par une conduite 15. The gas to be treated arrives at the washing column 1 and then in the permeator 2 at the pressure of the ammonia synthesis loop, ie 100 to 250 bars. It is rid of a large part of the ammonia which it contains in the apparatus 1, and of a large part of the hydrogen which it contains in the permeator 2, which produces under an average pressure of 70 a 80 bars a permeate consisting essentially of hydrogen and recycled to the synthesis installation via a pipe 15.

C'est donc un débit considérablement réduit qui est fourni a l'appareil d'épuration 3 par la conduite 13. Le gaz sortant, épuré du reste de l'ammoniac et de l'eau, passe a l'échangeur 4 via une conduite 16 et y est refroidi jusqu'à une température de condensation de tous les constituants autres que l'hydrogène, de l'ordre de -l900C.  It is therefore a considerably reduced flow rate which is supplied to the purification device 3 by the pipe 13. The outgoing gas, purified from the rest of the ammonia and water, passes to the exchanger 4 via a pipe 16 and is cooled there to a condensation temperature of all the constituents other than hydrogen, of the order of -1900C.

Le mélange refroidi est séparé dans le séparateur 5 en une phase vapeur constituée essentiellement du reliquat d'hydrogène et en un condensat constitué par un mélange d'azote, de méthane et d'argon. The cooled mixture is separated in the separator 5 into a vapor phase consisting essentially of the remainder of hydrogen and into a condensate consisting of a mixture of nitrogen, methane and argon.

Ce condensat, après détente å environ 2 bars absolus dans une vanne de détente 17, est introduit a mi-hauteur de la colonne 10. Cette dernière, qui est réfrigérée en tête -l900C et chauffée en cuve a -1SOOC, produit en cuve du méthane liquide et en azote un mélange azote-argon. This condensate, after expansion to approximately 2 bar absolute in an expansion valve 17, is introduced halfway up the column 10. The latter, which is refrigerated at the head -1900C and heated in tank at -1SOOC, produced in tank of liquid methane and nitrogen a nitrogen-argon mixture.

Ce mélange est envoyé a mi-hauteur de la colonne 11. Celle-ci, réfrigérée en tête å -19O0C et chauffée en cuve a -180iC, produit en tête un courant d'azote et en cuve de l'argon liquide, évacué par une conduite 18.  This mixture is sent halfway up column 11. The latter, refrigerated at the head at -19O0C and heated in tank at -180iC, produces a stream of nitrogen at the head and in the tank the liquid argon, evacuated by conduct 18.

L'azote est réchauffé a contre-courant du gaz traite dans l'échangeur 4, comprimé par le compresseur 6 jusqu'a 30 a 50 bars, puis refroidi et condensé dans l'échangeur 4. L'azote liquide ainsi produit est comprimé par la pompe 8 a la haute pression de l'installation et mélangé a l'hydrogène gazeux issu du séparateur 5. L'ensemble est vaporise dans l'échangeur 4 et réchauffé a la température ambiante, pour fournir un mélange gazeux azote-hydrogene qui est recyclé par une conduite 19 a l'étage approprié du compresseur de l'installation de synthèse d'ammoniac. The nitrogen is heated against the flow of the treated gas in the exchanger 4, compressed by the compressor 6 to 30 to 50 bars, then cooled and condensed in the exchanger 4. The liquid nitrogen thus produced is compressed by the pump 8 at the high pressure of the installation and mixed with the gaseous hydrogen coming from the separator 5. The whole is vaporized in the exchanger 4 and warmed up to room temperature, to provide a nitrogen-hydrogen gas mixture which is recycled through a line 19 to the appropriate stage of the compressor of the ammonia synthesis installation.

Comme indiqué sur la figure 1, une partie de l'azote comprimé en 6 est turbinée en 7 puis envoyée a l'aspiration du compresseur 6 afin de fournir l'appoint de frigories nécessaires. De plus, le méthane liquide produit par la colonne 10 est lui aussi vaporisé puis réchauffé dans l'échangeur 4 avant d'être acheminé par la conduite 14 a la bouteille d'adsorption 12 a régénérer, puis évacué au réseau "fuel gas" par une conduite 20. As indicated in FIG. 1, part of the nitrogen compressed at 6 is turbinated at 7 and then sent to the suction of the compressor 6 in order to supply the necessary frigories. In addition, the liquid methane produced by the column 10 is also vaporized and then reheated in the exchanger 4 before being conveyed via line 14 to the adsorption bottle 12 to be regenerated, then evacuated to the "fuel gas" network by a pipe 20.

L'élimination d'hydrogène assurée par le perméateur 2 permet de réduire considérablement l'investissement et le court de fonctionnement correspondant a l'appareil 3 et a la partie cryogénique 4 à 9 de l'installation. The elimination of hydrogen provided by the permeator 2 makes it possible to considerably reduce the investment and the operating shortage corresponding to the device 3 and to the cryogenic part 4 to 9 of the installation.

En variante, comme représenté a la figure 2, le perméateur peut etre monté en amont de l'appareil 1 et, par suite, être alimenté directement par le gaz de purge traiter, le résidu de la perméation étant envoyé a la base de la colonne de lavage 1. Ceci permet de réduire également les dimensions de cet appareil 1, ceci d'autant plus que comme les membranes de séparation d'hydrogène sont généralement relativement perméable à l'ammoniac, c'est un mélange hydrogène-ammoniac qui constitue le perméat. Le reste de l'installation est identique å celui de la figure 1. Alternatively, as shown in Figure 2, the permeator can be mounted upstream of the device 1 and, therefore, be supplied directly by the purge gas treated, the residue of the permeation being sent to the base of the column washing 1. This also makes it possible to reduce the dimensions of this device 1, all the more so since as the hydrogen separation membranes are generally relatively permeable to ammonia, it is a hydrogen-ammonia mixture which constitutes the permeate. The rest of the installation is identical to that of Figure 1.

La variante de la figure 3 ne diffère de la figure 1 que par l'appareil 1A de traitement primaire : au lieu d'éliminer l'ammoniac par lavage a l'eau, on refroidit et on condense partiellement le gaz de purge dans un échangeur de chaleur indirect 21, on Separe les phases liquide (essentiellement ammoniac) et vapeur dans un ne#arateur 22, on détend la phase vapeur dans une turbine 23 jusqu'a une pression moyenne de l'ordre de 70 a 80 bars, on sépare de nouveau les phases liquide (essentiellement ammoniac) et vapeur dans un second séparateur 24, et l'on réchauffe la phase vapeur dans l'échangeur 21, a contre-courant du gaz de départ, avant de l'introduire dans l'espace haute pression du perméateur 2.Ce dernier fournit donc de l'hydrogène basse pression (sous 30 a 50 bars) dans la conduite 15 et le mélange restant, traité dans le reste de l'installation, par la conduite 13. L'ammoniac liquide recueilli dans les séparateurs 22 et 24 est évacué, après détente, par une conduite 25. The variant of FIG. 3 differs from FIG. 1 only in the primary treatment apparatus 1A: instead of removing the ammonia by washing with water, the purge gas is cooled and partially condensed in an exchanger indirect heat 21, the liquid (mainly ammonia) and vapor phases are separated in a ne # arator 22, the vapor phase is expanded in a turbine 23 to an average pressure of the order of 70 to 80 bars, separated again the liquid (essentially ammonia) and vapor phases in a second separator 24, and the vapor phase is heated in the exchanger 21, against the flow of the starting gas, before introducing it into the upper space permeator pressure 2. The latter therefore supplies low pressure hydrogen (at 30 to 50 bars) in line 15 and the remaining mixture, treated in the rest of the installation, through line 13. The liquid ammonia collected in the separators 22 and 24 is discharged, after expansion, by a cond see 25.

Cette variante conduit a une séparation économique de l'ammoniac, de l'argon, de l'hydrogène et de l'azote, mais nécessite une recompression de l'hydrogène produit en basse pression. This variant leads to an economic separation of ammonia, argon, hydrogen and nitrogen, but requires recompression of the hydrogen produced at low pressure.

On retrouve l'appareil lA dans la variante de la figure 4, avec cette différence que la conduite 13 est directement reliée a la partie supérieure du séparateur 24 via l'échangeur 21. Le perméatour 2 est monté entre l'appareil d'épuration 3 et l'échangeur 4 et est alimenté, via la conduite 16, par le gaz débarrassé de l'ammoniac et de l'eau Z il fournit donc un perméat constitué essentiellement d'hydrogène sous la basse pression de 30 a 50 bars, et un résidu sous la pression moyenne précitée, ce résidu subissant la suite du traitement (refroidissement, condensation, distillation). We find the device 1A in the variant of FIG. 4, with the difference that the pipe 13 is directly connected to the upper part of the separator 24 via the exchanger 21. The permeateour 2 is mounted between the purification device 3 and the exchanger 4 and is supplied, via line 16, by the gas freed from ammonia and water Z, it therefore provides a permeate consisting essentially of hydrogen under low pressure from 30 to 50 bars, and a residue under the above-mentioned average pressure, this residue undergoing further treatment (cooling, condensation, distillation).

La partie cryogénique de l'installation est analogue a celle de la figure 1, ceci près que la pompe 8 délivre de l'azote liquide sous deux pressions différentes : d'une part sous la moyenne pression, ce courant étant mélangé J la vapeur issue du séparateur 5, et d'autre part, après détente dans une vanne de détente 26, sous la basse pression, ce courant étant mélangé avec le perméat précité préalablement refroidi dans l'échangeur 4. Ainsi, on net a profit la séparation d'hydrogène par perméation pour diminuer la pression partielle de l'azote vaporiser dans l'échangeur 4, ce qui favorise la réfrigération de cet échangeur. The cryogenic part of the installation is similar to that of FIG. 1, except that the pump 8 delivers liquid nitrogen under two different pressures: on the one hand under medium pressure, this current being mixed with the steam issuing of the separator 5, and on the other hand, after expansion in an expansion valve 26, under the low pressure, this current being mixed with the above-mentioned permeate previously cooled in the exchanger 4. Thus, the separation of hydrogen by permeation to reduce the partial pressure of the nitrogen vaporize in the exchanger 4, which promotes refrigeration of this exchanger.

On remarque qu'avec cet agencement, l'installation fournit deux mélanges azote-hydrogene, respectivement sous la moyenne pression et sous la basse pression, lesquels sont recyclés via des conduites 19,19A a des étages correspondants du compresseur de l'installation de synthèse d'ammoniac.  It is noted that with this arrangement, the installation supplies two nitrogen-hydrogen mixtures, respectively under medium pressure and under low pressure, which are recycled via pipes 19.19A to corresponding stages of the compressor of the synthesis installation. ammonia.

L'installation représentée a la figure 5 ne diffère de celle de la figure 4 que sous deux aspects - d'une part, le traitement primaire d'élimination d'ammoniac, en amont de l'appareil d'épuration 3, est un lavage a l'eau : le gaz de départ passe dans une colonne de lavage 1 identique celle de la figure 1, et c'est le gaz lave, soutiré en tête de cette colonne, qui alimente la conduite 13 - d'autre part, la pompe 8 refoule l'azote liquide sous une seule pression qui est la moyenne pression du permet issu du permeateur 2. The installation represented in FIG. 5 differs from that of FIG. 4 only in two aspects - on the one hand, the primary treatment for removing ammonia, upstream of the purification device 3, is a washing in water: the starting gas passes through a washing column 1 identical to that of FIG. 1, and it is the washing gas, drawn off at the top of this column, which feeds line 13 - on the other hand, the pump 8 delivers liquid nitrogen under a single pressure which is the medium pressure of the permit from permeator 2.

L'azote liquide refoulé est mélangé, au bout froid de l'échangeur 4, d'une part a ce permet préalablement refroidi dans l'échangeur, d'autre part a la vapeur issue du séparateur 5, détendue a la moyenne pression dans une vanne de détente 27. Il s'ensuit que l'installation fournit un mélange H2/N2 sous la moyenne pression seulement, par la conduite 19.  The discharged liquid nitrogen is mixed, at the cold end of the exchanger 4, on the one hand so that it is previously cooled in the exchanger, on the other hand with the vapor coming from the separator 5, expanded at medium pressure in a expansion valve 27. It follows that the installation supplies an H2 / N2 mixture under medium pressure only, via line 19.

Claims (7)

REVENDICATIONS 1. Procédé de récupération de l'hydrogène, de l'azote et de l'argon contenus dans un gaz de purge d'une installation de synthèse d'ammoniac1 du type comprenant un traitement primaire (1 ; 1A) pour éliminer l'essentiel de l'ammoniac, une épuration par adsorption (3) pour éliminer le reste de l'ammoniac et l'eau, une condensation partielle (4) pour séparer l'hydrogène, et une distillation du condensat (9) pour séparer l'azote, l'argon et le méthane, l'hydrogène et l'azote ainsi séparés étant recycles au compresseur de l'installation de synthèse d'ammoniac, caractérisé en ce qu'il comprend une étape de séparation d'hydrogène par perméation (2) en amont de l'étape de condensation (4). 1. Method for recovering the hydrogen, nitrogen and argon contained in a purge gas from an ammonia synthesis installation1 of the type comprising a primary treatment (1; 1A) to eliminate the essential ammonia, purification by adsorption (3) to remove the rest of the ammonia and water, partial condensation (4) to separate the hydrogen, and distillation of the condensate (9) to separate the nitrogen , argon and methane, hydrogen and nitrogen thus separated being recycled to the compressor of the ammonia synthesis installation, characterized in that it comprises a step of separation of hydrogen by permeation (2) upstream of the condensation stage (4). 2. Procédé suivant la revendication 1, caractérisé en ce qu'on effectue l'étape de perméation (2) avant le traitement primaire (1). 2. Method according to claim 1, characterized in that the permeation step (2) is carried out before the primary treatment (1). 3. Procédé suivant la revendication 1, caractérisé en ce qu'on effectue- ltetape de perméation (2) entre le traitement primaire (1) et l'étape d'épuration (3). 3. Method according to claim 1, characterized in that the permeation step (2) is carried out between the primary treatment (1) and the purification step (3). 4. Procédé suivant la revendication 1, caractérisé en ce qu'on effectue l'étape de perméation (2) entre l'étape d'épuration (3) et l'étape de condensation partielle (4 > .  4. Method according to claim 1, characterized in that the permeation step (2) is carried out between the purification step (3) and the partial condensation step (4>. 5. Procédé suivant la revendication 4, caractérise en ce qu'on liquéfie l'azote issu de la distillation, et l'on refroidit le mélange traité par vaporisation de l'azote liquide ainsi obtenu auquel on a ajouté une partie au moins du permeat de l'étape de perméation (2) et/ou la vapeur issue de l'étape de condensation partielle (4). 5. Method according to claim 4, characterized in that the nitrogen from the distillation is liquefied, and the treated mixture is cooled by vaporization of the liquid nitrogen thus obtained to which at least part of the permeat has been added from the permeation step (2) and / or the vapor from the partial condensation step (4). 6. Installation de récupération de l'hydrogène, de l'azote et de l'argon contenus dans un gaz de purge d'une installation de synthèse d'axooniac, du type comprenant un appareil de traitement primaire (1 ; lA > destiné éliminer l'essentiel de 1'ammoniac, un appareil d'épuration par adsorption (3) destiné a éliminer le reste de l'ammoniac et l'eau, un échangeur de chaleur indirect (4) destiné condenser l'ensemble des constituants restants sauf l'hydrogène, un appareil de distillation du condensat (9) destiné a séparer l'azote, l'argon et le méthane, et des moyens pour recycler l'azote et l'hydrogène au compresseur de l'installation de synthèse d'ammoniac, caractérisée en cè qu'elle comprend un perméateur (2) en amont de l'échangeur de chaleur (4). 6. Installation for recovering the hydrogen, nitrogen and argon contained in a purge gas from an axooniac synthesis installation, of the type comprising a primary treatment apparatus (1; lA> intended to eliminate the main part of the ammonia, an adsorption purification device (3) intended to remove the rest of the ammonia and the water, an indirect heat exchanger (4) intended to condense all of the remaining constituents except the hydrogen, a condensate distillation apparatus (9) for separating nitrogen, argon and methane, and means for recycling nitrogen and hydrogen to the compressor of the ammonia synthesis installation, characterized in that it includes a permeator (2) upstream of the heat exchanger (4). 7. Installation suivant la revendication 6, caractérisée en ce que l'échangeur de chaleur (4) est muni de moyens (6) pour liquéfier l'azote issu de l'appareil de distillation (9), de moyens pour ajouter à l'azote liquide ainsi obtenu de l'hydrogène résultant de la condensation partielle et/ou issu du perméateur (2), et de moyens pour vaporiser le ou les mélanges azote-hydrogène a contre-courant du mélange refroidi par l'échangeur de chaleur.  7. Installation according to claim 6, characterized in that the heat exchanger (4) is provided with means (6) for liquefying the nitrogen from the distillation apparatus (9), means for adding to the liquid nitrogen thus obtained from the hydrogen resulting from partial condensation and / or from the permeator (2), and means for vaporizing the nitrogen-hydrogen mixture (s) against the flow of the mixture cooled by the heat exchanger.
FR8811880A 1988-09-12 1988-09-12 Process and plant for treating a purge gas from an ammonium synthesis plant Granted FR2636543A1 (en)

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Cited By (5)

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EP0616834A1 (en) * 1993-03-18 1994-09-28 PERMEA, Inc. Process for cooling the feed gas to gas separation systems
FR2731163A1 (en) * 1995-03-03 1996-09-06 Air Liquide PROCESS AND INSTALLATION FOR SEPARATING A GAS MIXTURE BY PERMEATION
US6161397A (en) * 1998-08-12 2000-12-19 Air Products And Chemicals, Inc. Integrated cryogenic and non-cryogenic gas mixture separation
EP1278036A1 (en) * 2001-07-18 2003-01-22 Air Products And Chemicals, Inc. Cryogenic hydrogen and carbon monoxide production using an expander fed by the permeat of a membrane separation unit
CN105174288A (en) * 2015-08-24 2015-12-23 河南心连心化肥有限公司 Synthetic ammonia waste gas recovering and utilizing device and recovering and utilizing method thereof

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US4180553A (en) * 1978-03-20 1979-12-25 Monsanto Company Process for hydrogen recovery from ammonia purge gases
DE3315930A1 (en) * 1982-07-29 1984-03-01 Linde Ag, 6200 Wiesbaden Process and apparatus for separating a gas mixture
US4444571A (en) * 1983-03-07 1984-04-24 Bend Research, Inc. Energy-efficient process for the stripping of gases from liquids

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4180553A (en) * 1978-03-20 1979-12-25 Monsanto Company Process for hydrogen recovery from ammonia purge gases
DE3315930A1 (en) * 1982-07-29 1984-03-01 Linde Ag, 6200 Wiesbaden Process and apparatus for separating a gas mixture
US4444571A (en) * 1983-03-07 1984-04-24 Bend Research, Inc. Energy-efficient process for the stripping of gases from liquids

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0616834A1 (en) * 1993-03-18 1994-09-28 PERMEA, Inc. Process for cooling the feed gas to gas separation systems
FR2731163A1 (en) * 1995-03-03 1996-09-06 Air Liquide PROCESS AND INSTALLATION FOR SEPARATING A GAS MIXTURE BY PERMEATION
WO1996027427A1 (en) * 1995-03-03 1996-09-12 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method and apparatus for the permeation separation of a gas mixture
US6161397A (en) * 1998-08-12 2000-12-19 Air Products And Chemicals, Inc. Integrated cryogenic and non-cryogenic gas mixture separation
EP1278036A1 (en) * 2001-07-18 2003-01-22 Air Products And Chemicals, Inc. Cryogenic hydrogen and carbon monoxide production using an expander fed by the permeat of a membrane separation unit
US6568206B2 (en) 2001-07-18 2003-05-27 Air Products And Chemicals, Inc. Cryogenic hydrogen and carbon monoxide production with membrane permeate expander
CN105174288A (en) * 2015-08-24 2015-12-23 河南心连心化肥有限公司 Synthetic ammonia waste gas recovering and utilizing device and recovering and utilizing method thereof

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