EP3058296B1 - Method for denitrogenation of natural gas with or without helium recovery - Google Patents

Method for denitrogenation of natural gas with or without helium recovery Download PDF

Info

Publication number
EP3058296B1
EP3058296B1 EP14799510.4A EP14799510A EP3058296B1 EP 3058296 B1 EP3058296 B1 EP 3058296B1 EP 14799510 A EP14799510 A EP 14799510A EP 3058296 B1 EP3058296 B1 EP 3058296B1
Authority
EP
European Patent Office
Prior art keywords
column
gas
natural gas
turbine
sent
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.)
Active
Application number
EP14799510.4A
Other languages
German (de)
French (fr)
Other versions
EP3058296A2 (en
Inventor
Alain Briglia
Selim CHOUIK
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
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Priority to PL14799510T priority Critical patent/PL3058296T3/en
Publication of EP3058296A2 publication Critical patent/EP3058296A2/en
Application granted granted Critical
Publication of EP3058296B1 publication Critical patent/EP3058296B1/en
Priority to HRP20180610TT priority patent/HRP20180610T1/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

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
    • 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
    • F25J3/0209—Natural gas or substitute natural 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
    • 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
    • F25J3/0257—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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
    • F25J2200/06—Processes or apparatus using separation by rectification in a dual pressure main column system in a classical double column flow-sheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/08—Cold compressor, i.e. suction of the gas at cryogenic temperature and generally without afterstage-cooler
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/60—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being hydrocarbons or a mixture of hydrocarbons
    • 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
    • F25J2235/60—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being (a mixture of) hydrocarbons
    • 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
    • F25J2240/40—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval

Definitions

  • the present invention applies to denitrogenation processes of natural gas with or without helium recovery according to the preamble of claim 1 and known from the document US-A-4,758,258 .
  • the exploited natural gas fields contain more and more nitrogen. This is particularly due to the depletion and scarcity of fields rich enough that no enrichment treatment is necessary before the marketing of gas.
  • Unconventional resources such as shale gas also have the same problem: to make them marketable, it may be necessary to increase their calorific value by means of a pretreatment which consists of de-nitrogenising the raw gas.
  • US-A-4778498 describes a double column used for denitrogenation of natural gas.
  • Natural gas denitrogen units generally treat gases that come directly from wells at high pressure. After denaturing, the treated gas must be returned to the network, often at a pressure close to its inlet pressure.
  • the denitrogenation of natural gas uses cryogenic distillation techniques that take place at lower pressures than source pressures.
  • the sources can be at pressures of the order of 60 to 80 bara, while the cryogenic separation is carried out at pressures ranging from 30 bara to a pressure slightly above atmospheric pressure.
  • nitrogen purified natural gas is produced at low pressure and must be pumped and / or compressed to be introduced into the network.
  • the nitrogen-purified natural gas can be produced at different pressure levels at the outlet of the cold box.
  • the different streams are then compressed by external compression until the desired pressure is reached.
  • distillation at pressures greater than 12 bara is generally not well suited to the use of structured packings because of the "washing machine” phenomena, related to the approximation of the gas and liquid densities passing through the columns, which requires the use of trays for these pressure levels.
  • the invention consists in valuing the expansion of the natural gas in the different turbines of the process, using it to effect cold compression.
  • it may be product compression (typically natural gas purified by nitrogen).
  • it is the compression of a nitrogen enriched gas from a column of the column system. For example, the compression of the gas at the top of the high pressure column of a double column process makes it possible to reduce the pressure of this column.
  • the invention will be described in more detail with reference to the Figures 1 to 3 among which only the figure 3 illustrates a process according to the invention.
  • the process is carried out in an isolated cold box which contains an exchange line 1 and a double column 2,3 comprising a first column 2 operating at between 10 and 30 bara and a second column 3 operating at between 0.8 and 3 bara.
  • the first column 2 is thermally connected to the second column 3 by means of a vaporizer-condenser 5.
  • the exchange line comprises at least one heat exchanger, preferably brazed aluminum plates and fins.
  • the natural gas 10 which is generally at a pressure greater than 35 bara, cools in the exchange line 1.
  • a portion 11 of the natural gas representing between 1 and 80% of the gas to be separated, preferably between 5 and 55%, or even between 25 and 35% of the gas to be separated, is withdrawn from the exchange line 1 and is expanded in gaseous form in an expansion turbine 7 which produces a fluid that is sent to the bottom of the first column to separate.
  • the remainder of the natural gas 12 continues cooling in the exchange line where it is condensed, then is expanded in a flash valve before being sent in liquid form to the first column.
  • column 2 separates the gas natural in a liquid enriched methane 21 in the bottom of the column and a nitrogen-enriched gas at the top of the column.
  • the gas is used to heat the vaporizer-condenser 5 where it condenses and reflux at the top of the column 2.
  • the bottom liquid cools in a subcooler 4 and is expanded to be sent to an intermediate level of the second column 3.
  • An intermediate liquid 23 of the first column 2 is subcooled, expanded and sent to the top of the second column 3.
  • the waste nitrogen 18 is withdrawn at the top of the column and is heated in the exchangers 4.1.
  • Incondensable gases enriched in helium and nitrogen 17 leave the vaporizer 5 and heat up in the exchangers 4.1.
  • the methane-enriched liquid 13 of the second column 3 is withdrawn in the tank, pumped at high pressure by means of the pump 6, subcooled and then divided as flow 14 into three fractions.
  • a fraction 15A vaporizes in the exchange line 1 at the outlet pressure of the pump 6.
  • the fractions 15, 15B are expanded at different pressures from each other by valves and each vaporizes in the line exchange at a different vaporization pressure.
  • the fraction 15 leaves the exchange line as the gas flow 16.
  • the liquid 14 is divided in the same manner but the liquid 15 vaporizes in the exchange line 1, leaves it, is compressed in a cold in a CBP booster before being returned to the exchange line 1 to continue its warming.
  • This booster CBP values the energy of the turbine 7.
  • the liquids produced by the division of the liquid 14 vaporize in the same way as in the Figure 1 .
  • the nitrogen-enriched gas from the top of the first column 2 is compressed to a pressure of 17 to 30 bara in a cold booster CB1 having an inlet temperature generally below -150 ° C.
  • the compressed nitrogen serves to heat the vaporizer 5 where it condenses into a fluid 27 is expanded in a valve and returned to the top of the column 2.
  • the first and second columns can be replaced by a single column.
  • Natural gas to be treated 10 Natural gas to be treated, 11 Natural gas to be treated to turbine, 12 Natural gas to treat to expansion, 13 Low pressure liquid methane, 14 High pressure liquid methane, 15 Medium pressure liquid methane, 16 Medium pressure methane gas, 17 Mixture of nitrogen and helium, 18 Residual nitrogen.

Landscapes

  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

La présente invention s'applique aux procédés de déazotation de gaz naturel avec ou sans récupération d'hélium conformément au préambule de la revendication 1 et connu du document US-A-4 758 258 . Les gisements de gaz naturel exploités contiennent de plus en plus d'azote. Ceci s'explique notamment par l'épuisement et la raréfaction des champs suffisamment riches pour qu'aucun traitement d'enrichissement ne soit nécessaire avant la commercialisation du gaz.The present invention applies to denitrogenation processes of natural gas with or without helium recovery according to the preamble of claim 1 and known from the document US-A-4,758,258 . The exploited natural gas fields contain more and more nitrogen. This is particularly due to the depletion and scarcity of fields rich enough that no enrichment treatment is necessary before the marketing of gas.

Il est fréquent que ces sources de gaz naturel contiennent également de l'hélium. Celui-ci peut être valorisé en effectuant une pré-concentration, avant traitement final et liquéfaction.It is common for these natural gas sources to also contain helium. This can be valorized by performing a pre-concentration, before final treatment and liquefaction.

Les ressources non conventionnelles telles que les gaz de schiste, ont aussi la même problématique : pour les rendre commercialisable, il peut s'avérer nécessaire d'augmenter leur pouvoir calorifique au moyen d'un prétraitement qui consiste à déazoter le gaz brut.Unconventional resources such as shale gas also have the same problem: to make them marketable, it may be necessary to increase their calorific value by means of a pretreatment which consists of de-nitrogenising the raw gas.

US-A -4778498 décrit une double colonne utilisée pour une déazotation de gaz naturel. US-A-4778498 describes a double column used for denitrogenation of natural gas.

Il est connu de «Nitrogen Removal from Natural Gas » de M. Streich donnée à l'ICR12 à Madrid en 1967 d'utiliser une turbine pour détendre le gaz naturel à séparer dans une double colonne de déazotation.It is known to Mr. Streich's "Nitrogen Removal from Natural Gas" given to ICR12 in Madrid in 1967 to use a turbine to relax the natural gas to be separated in a double denitrogenation column.

Les unités de déazotation de gaz naturel traitent en général des gaz qui proviennent directement des puits à une pression élevée. Après déazotation le gaz traité doit être remis au réseau, souvent à une pression proche de sa pression d'entrée.Natural gas denitrogen units generally treat gases that come directly from wells at high pressure. After denaturing, the treated gas must be returned to the network, often at a pressure close to its inlet pressure.

La déazotation de gaz naturel, dans la majeure partie des cas, fait appel à des techniques de distillation cryogénique qui ont lieu à des pressions plus basses que les pressions des sources. Par exemple, les sources peuvent être à des pressions de l'ordre de 60 à 80 bara, alors que la séparation cryogénique s'effectue à des pressions variant de 30 bara à une pression légèrement supérieure à la pression atmosphérique. Généralement, le gaz naturel épuré en azote est produit à basse pression et doit être pompé et/ou comprimé pour être introduit dans le réseau.In most cases, the denitrogenation of natural gas uses cryogenic distillation techniques that take place at lower pressures than source pressures. For example, the sources can be at pressures of the order of 60 to 80 bara, while the cryogenic separation is carried out at pressures ranging from 30 bara to a pressure slightly above atmospheric pressure. Typically, nitrogen purified natural gas is produced at low pressure and must be pumped and / or compressed to be introduced into the network.

Afin d'adapter les bilans thermiques et énergétiques et de minimiser les coûts opératoires de l'unité, le gaz naturel épuré en azote peut être produit à différents niveaux de pression en sortie de boite froide. Les différents flux sont ensuite comprimés par compression externe jusqu'à atteindre la pression désirée.In order to adapt the thermal and energy balances and to minimize the operating costs of the unit, the nitrogen-purified natural gas can be produced at different pressure levels at the outlet of the cold box. The different streams are then compressed by external compression until the desired pressure is reached.

De plus, la distillation à des pressions supérieures à 12 bara n'est généralement pas bien adaptée à l'utilisation de garnissages structurés à cause des phénomènes de « lessiveuse », liés au rapprochement des densités gaz et liquide transitant par les colonnes, ce qui impose l'utilisation de plateaux pour ces niveaux de pressions.In addition, distillation at pressures greater than 12 bara is generally not well suited to the use of structured packings because of the "washing machine" phenomena, related to the approximation of the gas and liquid densities passing through the columns, which requires the use of trays for these pressure levels.

L'invention consiste à valoriser la détente du gaz naturel dans les différentes turbines du procédé, en l'utilisant pour effectuer de la compression froide. Selon une alternative non couverte par l'invention il peut s'agir de la compression de produit (typiquement du gaz naturel épuré en azote). Conformément à l'invention il s'agit de la compression d'un gaz enrichi en azote provenant d'une colonne du système de colonne. Par exemple, la compression du gaz en tête de colonne haute pression d'un procédé à double colonne permet de diminuer la pression de cette colonne.The invention consists in valuing the expansion of the natural gas in the different turbines of the process, using it to effect cold compression. According to an alternative not covered by the invention it may be product compression (typically natural gas purified by nitrogen). According to the invention it is the compression of a nitrogen enriched gas from a column of the column system. For example, the compression of the gas at the top of the high pressure column of a double column process makes it possible to reduce the pressure of this column.

Un tel procédé peut notamment permettre de :

  • Améliorer les coûts opératoires en optimisant la consommation énergétique ;
  • Réduire l'investissement ;
  • Améliorer la distillation ;
  • Le cas échéant, améliorer le rendement d'extraction de l'hélium.
Such a method can notably make it possible to:
  • Improve operating costs by optimizing energy consumption;
  • Reduce investment
  • Improve distillation
  • If necessary, improve the extraction efficiency of helium.

Selon un objet de l'invention, il est prévu un procédé de déazotation de gaz naturel par distillation selon la revendication 1.According to one object of the invention, there is provided a method of denitrogenation of natural gas by distillation according to claim 1.

Selon d'autres objets facultatifs :

  • une deuxième partie du gaz naturel se condense au moins partiellement et est envoyée sous forme au moins partiellement condensée à une colonne du système de colonnes.
  • le liquide enrichi en méthane soutiré d'une colonne du système est totalement ou partiellement pompé à un ou différents niveau(x) de pression avant d'être vaporisé dans la ligne d'échange.
  • le liquide enrichi en méthane, préalablement pompé, est divisé en au moins deux fractions, dont au moins une est détendue dans une vanne avant de se vaporiser dans la ligne d'échange.
  • le système comprend une première colonne opérant à une première pression, une deuxième colonne opérant à une deuxième pression plus basse que la première pression, la deuxième colonne étant reliée thermiquement à la première colonne, le gaz naturel étant envoyé à la première colonne pour produire un liquide de cuve et un gaz de tête, au moins une partie du liquide de cuve est envoyé à la deuxième colonne, au moins une partie du gaz de tête servant à chauffer la cuve de la deuxième colonne, le gaz enrichi en azote est soutiré de la tête de la deuxième colonne et le liquide enrichi en méthane est soutiré de la cuve de la deuxième colonne et le gaz détendu dans la turbine est envoyé à la première colonne sous forme gazeuse.
  • un liquide intermédiaire de la première colonne est détendu et envoyé à la deuxième colonne à un niveau intermédiaire ou en tête de celle-ci.
  • entre 1 et 80%du gaz à séparer, de préférence entre 5 et 55%, voire entre 25 et 35% du gaz à séparer, est détendue sous forme gazeuse dans la turbine de détente
  • l'au moins une partie du gaz naturel refroidie dans l'échangeur de chaleur et envoyée à la turbine reste gazeuse pendant son refroidissement en amont de la turbine.
  • la partie de gaz naturel destinée à la turbine est soutirée à un niveau intermédiaire de l'échangeur de chaleur.
  • la deuxième partie de gaz naturel se refroidit jusqu'au bout froid de l'échangeur de chaleur.
According to other optional objects:
  • a second portion of the natural gas condenses at least partially and is sent in at least partially condensed form to a column of the column system.
  • the methane-enriched liquid withdrawn from a column of the system is totally or partially pumped at one or more pressure level (s) before being vaporized in the exchange line.
  • the methane-enriched liquid, previously pumped, is divided into at least two fractions, at least one of which is expanded in a valve before vaporizing in the exchange line.
  • the system comprises a first column operating at a first pressure, a second column operating at a second pressure lower than the first pressure, the second column being thermally connected to the first column, the natural gas being sent to the first column to produce a vessel liquid and a top gas, at least a portion of the vessel liquid is fed to the second column, at least a portion of the overhead gas for heating the vessel of the second column, the nitrogen-enriched gas is withdrawn from the head of the second column and the methane enriched liquid is withdrawn from the tank of the second column and the gas expanded in the turbine is sent to the first column in gaseous form.
  • an intermediate liquid of the first column is expanded and sent to the second column at an intermediate level or at the top thereof.
  • between 1 and 80% of the gas to be separated, preferably between 5 and 55%, or even between 25 and 35% of the gas to be separated, is expanded in gaseous form in the expansion turbine
  • the at least part of the natural gas cooled in the heat exchanger and sent to the turbine remains gaseous during its cooling upstream of the turbine.
  • the natural gas portion for the turbine is withdrawn at an intermediate level of the heat exchanger.
  • the second part of natural gas cools to the cold end of the heat exchanger.

L'invention sera décrite de manière plus détaillée en se référant aux figures 1 à 3 parmi lesquelles seule la figure 3 illustre un procédé selon l'invention. Dans tous les cas, le procédé s'effectue dans une boîte froide isolée qui contient une ligne d'échange 1 et une double colonne 2,3 comprenant une première colonne 2 opérant à entre 10 et 30 bara et une deuxième colonne 3 opérant à entre 0,8 et 3 bara. La première colonne 2 est reliée thermiquement à la deuxième colonne 3 au moyen d'un vaporiseur-condenseur 5. La ligne d'échange comprend au moins un échangeur de chaleur, de préférence en aluminium brasé à plaques et à ailettes.The invention will be described in more detail with reference to the Figures 1 to 3 among which only the figure 3 illustrates a process according to the invention. In all cases, the process is carried out in an isolated cold box which contains an exchange line 1 and a double column 2,3 comprising a first column 2 operating at between 10 and 30 bara and a second column 3 operating at between 0.8 and 3 bara. The first column 2 is thermally connected to the second column 3 by means of a vaporizer-condenser 5. The exchange line comprises at least one heat exchanger, preferably brazed aluminum plates and fins.

Dans toutes les figures, le gaz naturel 10, qui est généralement à une pression supérieure à 35 bara, se refroidit dans la ligne d'échange 1. A une température intermédiaire de celle-ci, une partie 11 du gaz naturel, représentant entre 1 et 80% du gaz à séparer, de préférence entre 5 et 55%, voire entre 25 et 35% du gaz à séparer, est soutiré de la ligne d'échange 1 et est détendue sous forme gazeuse dans une turbine de détente 7 qui produit un fluide qui est envoyé en cuve de la première colonne pour s'y séparer. Le reste du gaz naturel 12 poursuit son refroidissement dans la ligne d'échange où il est condensé, puis est détendu dans une vanne de détente avant d'être envoyé sous forme liquide à la première colonne. Alimentée par ces deux fluides, la colonne 2 sépare le gaz naturel en un liquide enrichi en méthane 21 en cuve de colonne et un gaz enrichi en azote en tête de colonne. Le gaz sert à réchauffer le vaporiseur-condenseur 5 où il se condense et assure le reflux en tête de la colonne 2. Le liquide de cuve se refroidit dans un sous-refroidisseur 4 et est détendu pour être envoyé à un niveau intermédiaire de la deuxième colonne 3. Un liquide intermédiaire 23 de la première colonne 2 est sous-refroidi, détendu et envoyé en tête de la deuxième colonne 3. L'azote résiduaire 18 est soutiré en tête de la colonne et se réchauffe dans les échangeurs 4,1.In all the figures, the natural gas 10, which is generally at a pressure greater than 35 bara, cools in the exchange line 1. At an intermediate temperature thereof, a portion 11 of the natural gas, representing between 1 and 80% of the gas to be separated, preferably between 5 and 55%, or even between 25 and 35% of the gas to be separated, is withdrawn from the exchange line 1 and is expanded in gaseous form in an expansion turbine 7 which produces a fluid that is sent to the bottom of the first column to separate. The remainder of the natural gas 12 continues cooling in the exchange line where it is condensed, then is expanded in a flash valve before being sent in liquid form to the first column. Powered by these two fluids, column 2 separates the gas natural in a liquid enriched methane 21 in the bottom of the column and a nitrogen-enriched gas at the top of the column. The gas is used to heat the vaporizer-condenser 5 where it condenses and reflux at the top of the column 2. The bottom liquid cools in a subcooler 4 and is expanded to be sent to an intermediate level of the second column 3. An intermediate liquid 23 of the first column 2 is subcooled, expanded and sent to the top of the second column 3. The waste nitrogen 18 is withdrawn at the top of the column and is heated in the exchangers 4.1.

Des gaz incondensables enrichis en hélium et azote 17 sortent du vaporiseur 5 et se réchauffent dans les échangeurs 4,1.Incondensable gases enriched in helium and nitrogen 17 leave the vaporizer 5 and heat up in the exchangers 4.1.

Dans la Figure 1, le liquide 13 enrichi en méthane de la deuxième colonne 3 est soutiré en cuve, pompé à haute pression au moyen de la pompe 6, sous-refroidi et puis divisé comme débit 14 en trois fractions. Une fraction 15A se vaporise dans la ligne d'échange 1 à la pression de sortie de la pompe 6. Les fractions 15,15B sont détendues à des pressions différentes l'une de l'autre par des vannes et chacune se vaporise dans la ligne d'échange à une pression de vaporisation différente. La fraction 15 sort de la ligne d'échange comme débit gazeux 16.In the Figure 1 , the methane-enriched liquid 13 of the second column 3 is withdrawn in the tank, pumped at high pressure by means of the pump 6, subcooled and then divided as flow 14 into three fractions. A fraction 15A vaporizes in the exchange line 1 at the outlet pressure of the pump 6. The fractions 15, 15B are expanded at different pressures from each other by valves and each vaporizes in the line exchange at a different vaporization pressure. The fraction 15 leaves the exchange line as the gas flow 16.

Dans la Figure 2, le liquide 14 est divisé de la même manière mais le liquide 15 se vaporise dans la ligne d'échange 1, sort de celle-ci, est comprimé à froid dans un surpresseur CBP avant d'être renvoyé dans la ligne d'échange 1 pour poursuivre son réchauffement. Ce surpresseur CBP valorise l'énergie de la turbine 7.In the Figure 2 the liquid 14 is divided in the same manner but the liquid 15 vaporizes in the exchange line 1, leaves it, is compressed in a cold in a CBP booster before being returned to the exchange line 1 to continue its warming. This booster CBP values the energy of the turbine 7.

Dans la Figure 3, qui illustre un procédé selon l'invention, les liquides produits par la division du liquide 14 se vaporisent de la même manière que dans la Figure 1. Par contre le gaz enrichi en azote 25 de la tête de la première colonne 2 est comprimé jusqu'à une pression de 17 à 30 bara dans un surpresseur froid CB1 ayant une température d'entrée généralement inférieure à -150°C. L'azote comprimé sert à chauffer le vaporiseur 5 où il se condense en un fluide 27 est détendu dans une vanne et renvoyé en tête de la colonne 2.In the Figure 3 , which illustrates a process according to the invention, the liquids produced by the division of the liquid 14 vaporize in the same way as in the Figure 1 . In contrast, the nitrogen-enriched gas from the top of the first column 2 is compressed to a pressure of 17 to 30 bara in a cold booster CB1 having an inlet temperature generally below -150 ° C. The compressed nitrogen serves to heat the vaporizer 5 where it condenses into a fluid 27 is expanded in a valve and returned to the top of the column 2.

Les première et deuxième colonnes peuvent être remplacées par une simple colonne.The first and second columns can be replaced by a single column.

Equipements:Facilities:

1 Ligne d'échange principal, 2 Première colonne, haute pression, 3 Deuxième colonne, basse pression 4 Sous-refroidisseur, 5 Vaporiseur condenseur, 6 Pompe de méthane, 7 Turbine de détente. CBP Surpresseur froid de production ; CBI Supresseur froid de fluide interne 1 main exchange line, 2 first column, high pressure, 3 second column, low pressure 4 subcooler, 5 condenser vaporizer, 6 methane pump, 7 expansion turbine. CBP Cold production booster; CBI Internal fluid cold suppressor

Fluides:fluids:

10 Gaz naturel à traiter, 11 Gaz naturel à traiter vers turbine, 12 Gaz naturel à traiter vers détente, 13 Méthane liquide basse pression , 14 Méthane liquide haute pression, 15 Méthane liquide moyenne pression, 16 Méthane gazeux moyenne pression, 17 Mixture d'azote et d' hélium, 18 Azote résiduaire. 10 Natural gas to be treated, 11 Natural gas to be treated to turbine, 12 Natural gas to treat to expansion, 13 Low pressure liquid methane, 14 High pressure liquid methane, 15 Medium pressure liquid methane, 16 Medium pressure methane gas, 17 Mixture of nitrogen and helium, 18 Residual nitrogen.

Claims (9)

  1. Method for denitrogenation of natural gas by distillation wherein:
    i) natural gas (11, 12) cooled in an exchange line (1) is separated in a system of columns including at least two columns (2, 3),
    ii) a nitrogen-enriched gas (18) is drawn from one column (3) of the system of columns and is heated in the exchange line,
    iii) a methane-enriched liquid (13) is drawn from one column (3) of the system of columns, pressurised and vaporised in the exchange line at at least one vaporisation pressure and at least one portion of the cooled natural gas expands in gaseous form in a turbine (7) and is sent to one column (2) of the system of columns in gaseous form characterised in that the methane-enriched liquid is vaporised in the exchange line at at least two vaporisation pressures, even three and characterised in that the energy provided by the turbine (7) is valorised in at least one compressor (CBI, CBP) that compresses a gas of the method, with the compressor having an input temperature less than the ambient temperature, even less than -150°C, with the compressor (CBI, CBP) being directly driven by the turbine (7) and with the gas of the method being a nitrogen-enriched gas (25) coming from a column (2) of the system of columns which is compressed in the compressor (CB1) and is then used to heat the tank of another column (3) of the system.
  2. Method according to claim 1 wherein a second portion (12) of the natural gas is condensed at least partially and is sent in the at least partially condensed form to one column (2) of the system of columns.
  3. Method according to one of the preceding claims wherein the methane-enriched liquid (13) drawn from a column (3) of the system is totally or partially pumped at one or different levels of pressure before being vaporised in the exchange line (1).
  4. Method according to claim 3 wherein the methane-enriched liquid (13), pumped beforehand, is divided into at least two fractions (15, 15A, 15B), of which at least one is expanded in a valve before being vaporised in the exchange line.
  5. Method according to one of the preceding claims wherein the system comprises a first column operating at a first pressure (2), a second column (3) operating at a second pressure that is lower than the first pressure, with the second column being thermally connected to the first column, with the natural gas (11,12) being sent to the first column in order to produce a tank liquid (13) and a head gas (18), at least one portion of the enriched tank liquid is sent to the second column, at least one portion of the head gas used to heat the tank of the second column, the nitrogen-enriched gas (18) is drawn from the head of the second column and the methane-enriched liquid is drawn from the tank of the second column and the gas expanded in the turbine (7) is sent to the first column in gaseous form.
  6. Method according to claim 5 wherein an intermediate liquid (23) of the first column (2) is expanded and sent to the second column (3) at an intermediate level or at the head of the latter.
  7. Method according to one of the preceding claims wherein the at least one portion of the natural gas cooled in the heat exchanger and sent to the turbine remains gaseous during the cooling thereof upstream from the turbine.
  8. Method according to one of the preceding claims wherein the portion of natural gas (11) intended for the turbine is drawn at an intermediate level of the heat exchanger.
  9. Method according to claim 8 wherein the second portion of natural gas is cooled to the cold end of the heat exchanger.
EP14799510.4A 2013-10-18 2014-10-14 Method for denitrogenation of natural gas with or without helium recovery Active EP3058296B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PL14799510T PL3058296T3 (en) 2013-10-18 2014-10-14 Method for denitrogenation of natural gas with or without helium recovery
HRP20180610TT HRP20180610T1 (en) 2013-10-18 2018-04-17 Method for denitrogenation of natural gas with or without helium recovery

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1360138A FR3012211B1 (en) 2013-10-18 2013-10-18 PROCESS FOR DEAZATING NATURAL GAS WITH OR WITHOUT RECOVERING HELIUM
PCT/FR2014/052606 WO2015055938A2 (en) 2013-10-18 2014-10-14 Method for denitrogenation of natural gas with or without helium recovery

Publications (2)

Publication Number Publication Date
EP3058296A2 EP3058296A2 (en) 2016-08-24
EP3058296B1 true EP3058296B1 (en) 2018-03-28

Family

ID=49998435

Family Applications (1)

Application Number Title Priority Date Filing Date
EP14799510.4A Active EP3058296B1 (en) 2013-10-18 2014-10-14 Method for denitrogenation of natural gas with or without helium recovery

Country Status (9)

Country Link
US (1) US10006699B2 (en)
EP (1) EP3058296B1 (en)
EA (1) EA034668B1 (en)
FR (1) FR3012211B1 (en)
HR (1) HRP20180610T1 (en)
MX (1) MX2016004800A (en)
PL (1) PL3058296T3 (en)
SA (1) SA516370968B1 (en)
WO (1) WO2015055938A2 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3121743B1 (en) 2021-04-09 2023-04-21 Air Liquide Process and apparatus for separating a mixture containing at least nitrogen and methane

Family Cites Families (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2557171A (en) * 1946-11-12 1951-06-19 Pritchard & Co J F Method of treating natural gas
JPS5420986A (en) * 1977-07-18 1979-02-16 Kobe Steel Ltd Method of equipment for separating air
US4331461A (en) * 1978-03-10 1982-05-25 Phillips Petroleum Company Cryogenic separation of lean and rich gas streams
US4357153A (en) * 1981-03-30 1982-11-02 Erickson Donald C Internally heat pumped single pressure distillative separations
US4710212A (en) 1986-09-24 1987-12-01 Union Carbide Corporation Process to produce high pressure methane gas
US4758258A (en) * 1987-05-06 1988-07-19 Kerr-Mcgee Corporation Process for recovering helium from a natural gas stream
US4936888A (en) * 1989-12-21 1990-06-26 Phillips Petroleum Company Nitrogen rejection unit
US4948405A (en) * 1989-12-26 1990-08-14 Phillips Petroleum Company Nitrogen rejection unit
US5692395A (en) * 1995-01-20 1997-12-02 Agrawal; Rakesh Separation of fluid mixtures in multiple distillation columns
DE10215125A1 (en) * 2002-04-05 2003-10-16 Linde Ag Process for removing nitrogen from a hydrocarbon-rich fraction containing nitrogen comprises compressing a partial stream of a previously heated nitrogen-rich fraction, cooling, condensing, and mixing with a nitrogen-rich feed
GB0220791D0 (en) * 2002-09-06 2002-10-16 Boc Group Plc Nitrogen rejection method and apparatus
GB0226983D0 (en) * 2002-11-19 2002-12-24 Boc Group Plc Nitrogen rejection method and apparatus
DE102009009477A1 (en) * 2009-02-19 2010-08-26 Linde Aktiengesellschaft Process for separating nitrogen
GB2455462B (en) * 2009-03-25 2010-01-06 Costain Oil Gas & Process Ltd Process and apparatus for separation of hydrocarbons and nitrogen
DE202009010874U1 (en) * 2009-08-11 2009-11-19 Linde Aktiengesellschaft Device for producing a gaseous print product by cryogenic separation of air
US20140060114A1 (en) * 2012-08-30 2014-03-06 Fluor Technologies Corporation Configurations and methods for offshore ngl recovery

Also Published As

Publication number Publication date
US10006699B2 (en) 2018-06-26
FR3012211A1 (en) 2015-04-24
FR3012211B1 (en) 2018-11-02
EA201690799A1 (en) 2016-08-31
PL3058296T3 (en) 2018-09-28
MX2016004800A (en) 2016-07-18
EA034668B1 (en) 2020-03-04
HRP20180610T1 (en) 2018-06-29
SA516370968B1 (en) 2020-10-20
US20160245584A1 (en) 2016-08-25
WO2015055938A3 (en) 2015-12-03
EP3058296A2 (en) 2016-08-24
WO2015055938A2 (en) 2015-04-23

Similar Documents

Publication Publication Date Title
JP4713548B2 (en) Natural gas liquefaction method and apparatus
RU2215952C2 (en) Method of separation of pressurized initial multicomponent material flow by distillation
US10113127B2 (en) Process for separating nitrogen from a natural gas stream with nitrogen stripping in the production of liquefied natural gas
CA2828179C (en) Method and apparatus for the liquefaction of co2
US20140083132A1 (en) Process for liquefaction of natural gas
US9903645B2 (en) Method for ethane liquefaction with demethanization
FR2885679A1 (en) METHOD AND INSTALLATION FOR SEPARATING LIQUEFIED NATURAL GAS
JP2009041017A (en) Method for removing nitrogen from condensed natural gas
EP1623172A1 (en) Method and system for the production of pressurized air gas by cryogenic distillation of air
CA2832096C (en) Method and apparatus for liquefying a co2-rich gas
WO2013135993A2 (en) Method and device for separating a mixture containing carbon dioxide by means of distillation
CN107295807A (en) Supply the device and method of liquid fuel gas
EP3058296B1 (en) Method for denitrogenation of natural gas with or without helium recovery
EP3058297A2 (en) Method and device for separating air by cryogenic distillation
FR2973485A1 (en) Method for separating air by cryogenic distillation in column system, involves withdrawing liquid containing specific mol percent of oxygen from bottom of low pressure column, where liquid is pressurized and vaporized to form gaseous oxygen
CA2885677A1 (en) Method and appliance for separating a mixture containing carbon dioxide by cryogenic distillation
FR2990748A1 (en) METHOD AND APPARATUS FOR DISTILLATION AT SUBAMBIAN TEMPERATURE
WO2022162041A1 (en) Method and apparatus for separating a flow rich in carbon dioxide by distillation to produce liquid carbon dioxide
FR3110223A1 (en) Process for extracting nitrogen from a stream of natural gas or bio-methane
FR3113606A3 (en) Nitrogen and methane separation process by cryogenic distillation
FR3128011A1 (en) Method and apparatus for cooling a CO2-rich flow
RU32583U1 (en) Installation of low-temperature separation of hydrocarbon gas
CA3220225A1 (en) Method and apparatus for the liquefaction of co2 by distillation
WO2012140381A2 (en) Method and apparatus for separating a feed gas
FR2987755A1 (en) Method for separating gas containing carbon dioxide and e.g. component, lighter than carbon dioxide by distillation, involves sending part of vaporized liquid to reboiler tank, and returning vaporized part of liquid to distillation column

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20160603

AK Designated contracting states

Kind code of ref document: A2

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

AX Request for extension of the european patent

Extension state: BA ME

DAX Request for extension of the european patent (deleted)
GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

INTG Intention to grant announced

Effective date: 20171201

RIN1 Information on inventor provided before grant (corrected)

Inventor name: BRIGLIA, ALAIN

Inventor name: CHOUIK, SELIM

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REG Reference to a national code

Ref country code: AT

Ref legal event code: REF

Ref document number: 983816

Country of ref document: AT

Kind code of ref document: T

Effective date: 20180415

REG Reference to a national code

Ref country code: HR

Ref legal event code: TUEP

Ref document number: P20180610

Country of ref document: HR

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

Free format text: LANGUAGE OF EP DOCUMENT: FRENCH

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 602014023072

Country of ref document: DE

REG Reference to a national code

Ref country code: HR

Ref legal event code: T1PR

Ref document number: P20180610

Country of ref document: HR

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180628

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

REG Reference to a national code

Ref country code: NL

Ref legal event code: MP

Effective date: 20180328

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG4D

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: RS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180629

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180628

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 5

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: ES

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: AL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SM

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

REG Reference to a national code

Ref country code: AT

Ref legal event code: MK05

Ref document number: 983816

Country of ref document: AT

Kind code of ref document: T

Effective date: 20180328

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180730

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602014023072

Country of ref document: DE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: AT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20190103

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

REG Reference to a national code

Ref country code: BE

Ref legal event code: MM

Effective date: 20181031

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181014

REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181031

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181031

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181031

REG Reference to a national code

Ref country code: HR

Ref legal event code: ODRP

Ref document number: P20180610

Country of ref document: HR

Payment date: 20190926

Year of fee payment: 6

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181014

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MK

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180328

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO

Effective date: 20141014

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180328

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180728

REG Reference to a national code

Ref country code: HR

Ref legal event code: ODRP

Ref document number: P20180610

Country of ref document: HR

Payment date: 20201009

Year of fee payment: 7

REG Reference to a national code

Ref country code: HR

Ref legal event code: ODRP

Ref document number: P20180610

Country of ref document: HR

Payment date: 20211007

Year of fee payment: 8

REG Reference to a national code

Ref country code: HR

Ref legal event code: ODRP

Ref document number: P20180610

Country of ref document: HR

Payment date: 20221010

Year of fee payment: 9

REG Reference to a national code

Ref country code: HR

Ref legal event code: ODRP

Ref document number: P20180610

Country of ref document: HR

Payment date: 20231005

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20231020

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: HR

Payment date: 20231005

Year of fee payment: 10

Ref country code: FR

Payment date: 20231026

Year of fee payment: 10

Ref country code: DE

Payment date: 20231020

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: PL

Payment date: 20231006

Year of fee payment: 10