FR3011320A1 - METHOD AND APPARATUS FOR SEPARATION BY CRYOGENIC DISTILLATION OF A MIXTURE COMPRISING HYDROGEN, CARBON MONOXIDE AND METHANE - Google Patents
METHOD AND APPARATUS FOR SEPARATION BY CRYOGENIC DISTILLATION OF A MIXTURE COMPRISING HYDROGEN, CARBON MONOXIDE AND METHANE Download PDFInfo
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- FR3011320A1 FR3011320A1 FR1359525A FR1359525A FR3011320A1 FR 3011320 A1 FR3011320 A1 FR 3011320A1 FR 1359525 A FR1359525 A FR 1359525A FR 1359525 A FR1359525 A FR 1359525A FR 3011320 A1 FR3011320 A1 FR 3011320A1
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- separation
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000926 separation method Methods 0.000 title claims abstract description 34
- 239000001257 hydrogen Substances 0.000 title claims abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 29
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical class [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910002091 carbon monoxide Inorganic materials 0.000 title claims abstract description 21
- 239000000203 mixture Substances 0.000 title claims abstract description 20
- 238000004821 distillation Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 title claims description 11
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 239000007789 gas Substances 0.000 claims abstract description 15
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 230000008016 vaporization Effects 0.000 claims description 10
- 238000009834 vaporization Methods 0.000 claims description 6
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000011144 upstream manufacturing Methods 0.000 claims description 5
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- F25J3/0233—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
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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
- F25J3/0204—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
- F25J3/0223—H2/CO mixtures, i.e. synthesis gas; Water gas or shifted synthesis gas
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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
- F25J3/0252—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
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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
- F25J3/0257—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
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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
- F25J3/0261—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of carbon monoxide
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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
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
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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
- 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
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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
- F25J2270/00—Refrigeration techniques used
- F25J2270/02—Internal refrigeration with liquid vaporising loop
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
Dans un procédé de séparation par distillation cryogénique d'un mélange d'hydrogène, de monoxyde de carbone et de méthane, le mélange (1) est refroidi et partiellement condensé, au moins une partie du liquide formé (15) est envoyé à une colonne d'épuisement (K1) pour produire un gaz de tête (21) enrichi en hydrogène et un liquide de cuve (19) appauvri en hydrogène, e liquide appauvri en hydrogène est divisé en une première et une deuxième portions, la première portion (29) est envoyé sous forme liquide à une colonne de séparation CO/ CH4 (K2), la deuxième portion (27) est vaporisée et envoyée sous forme gazeuse à la colonne de séparation CO/CH4 et on soutire un débit riche en méthane (41) en cuve de la colonne de séparation CO/CH4 et un débit riche en monoxyde de carbone (43) de la tête de la colonne de séparation CO/CH4.In a cryogenic distillation separation process of a mixture of hydrogen, carbon monoxide and methane, the mixture (1) is cooled and partially condensed, at least a portion of the formed liquid (15) is sent to a column for depletion (K1) to produce a hydrogen-enriched overhead gas (21) and a hydrogen-depleted reactor liquid (19), the hydrogen-depleted liquid is divided into first and second portions, the first portion (29) ) is sent in liquid form to a CO / CH4 separation column (K2), the second portion (27) is vaporized and sent in gaseous form to the CO / CH4 separation column and a methane-rich flow is withdrawn (41) in the tank of the CO / CH4 separation column and a carbon monoxide rich flow (43) of the head of the CO / CH4 separation column.
Description
La présente invention concerne un procédé et un appareil de séparation par distillation cryogénique d'un mélange d'hydrogène, de monoxyde de carbone et de méthane. Le mélange peut éventuellement contenir de l'azote ou d'autres impuretés (par exemple l'argon, l'éthane..). En cas de présence d'azote, l'appareil comprend éventuellement une colonne de déazotation, selon les puretés requises sur le produit (monoxyde de carbone).The present invention relates to a method and apparatus for separating cryogenic distillation of a mixture of hydrogen, carbon monoxide and methane. The mixture may optionally contain nitrogen or other impurities (eg argon, ethane, etc.). In case of presence of nitrogen, the apparatus optionally comprises a denitrogenation column, according to the purities required on the product (carbon monoxide).
Le procédé est un procédé du type condensation partielle utilisant une colonne d'épuisement (en anglais « flash column ») et une colonne de séparation CO/CH4. Il est connu de « Progress in H2/CO Low Temperature Separation » de Berninger, Linde Reports 44/1988 de détendre tout le liquide de cuve de la colonne d'épuisement et ensuite de le réchauffer avant l'envoyer à une colonne de séparation CO/CH4. « Industrial Gases Processing » de Hâring montre à la page 154 un procédé de condensation partielle où une partie du liquide de la colonne d'épuisement est envoyée directement à la colonne CO/CH4 sans avoir été réchauffée et le reste est détendu et ensuite réchauffé dans un échangeur de chaleur avant d'être envoyé à cette colonne. Les frigories du système viennent de la vaporisation du CO de cycle et de l'hydrogène qui se réchauffe.The process is a partial condensation type process using a flash column and a CO / CH4 separation column. It is known from Berninger's Progress in H2 / CO Low Temperature Separation, Linde Reports 44/1988 to relax all the liquid from the bottom of the exhaustion column and then heat it up before sending it to a CO separation column. / CH4. Hâring's Industrial Gases Processing shows on page 154 a partial condensation process where part of the liquid from the exhaustion column is sent directly to the CO / CH4 column without having been reheated and the rest is expanded and then reheated in a heat exchanger before being sent to this column. The frigories of the system come from the vaporization of the cycle CO and the hydrogen that heats up.
Un objet de la présente invention est de réduire les consommations énergétiques des solutions connues. Un autre objet de la présente invention est la réduction des écarts de température dans au moins un échangeur de l'appareil, en particulier en réduisant l'écart maximal, dans au moins un échangeur où des liquides se vaporisent, à une valeur inférieure à 17°C, voire à 25 13°C. Selon un objet de l'invention, il est prévu un procédé de séparation par distillation cryogénique d'un mélange d'hydrogène, de monoxyde de carbone et de méthane et éventuellement d'azote et/ou de l'argon et/ou de l'éthane dans lequel : i) le mélange est refroidi et partiellement condensé, 30 ii) au moins une partie du liquide formé est envoyé à une colonne d'épuisement pour produire un gaz de tête enrichi en hydrogène et un liquide de cuve appauvri en hydrogène, iii) le liquide appauvri en hydrogène est divisé en une première et une deuxième portions, la première portion est envoyé sous forme liquide à une colonne de séparation CO/CH4, la deuxième portion est vaporisée et envoyée sous forme gazeuse à la colonne de séparation CO/CH4, iv) on soutire un débit riche en méthane en cuve de la colonne de séparation CO/CH4 et un débit riche en monoxyde de carbone de la tête de la colonne de séparation CO/CH4. Selon d'autres aspects facultatifs : - on vaporise la deuxième portion à au moins deux pressions différentes, après l'avoir divisée en au moins deux fractions. - les pressions différentes sont comprises entre la pression de la colonne d'épuisement et la pression de la colonne de séparation CO/CH4. - on vaporise la deuxième portion par échange de chaleur avec le mélange qui se refroidit. - l'écart maximal de température dans l'échangeur de chaleur où se refroidit le mélange et où se vaporise la deuxième portion ne dépasse pas 17°C, voire 13°C. Selon un autre objet de l'invention, il est prévu un appareil de séparation par distillation cryogénique d'un mélange d'hydrogène, de monoxyde de carbone et de méthane et éventuellement d'azote et/ou de l'argon et/ou de l'éthane comprenant un séparateur de phases, une colonne d'épuisement, une colonne de séparation CO/CH4 et éventuellement une colonne de déazotation, un échangeur de chaleur, une conduite pour envoyer le mélange se refroidir dans l'échangeur de chaleur où il se condense partiellement, une conduite pour envoyer le mélange partiellement condensé de l'échangeur de chaleur au séparateur de phases, une conduite pour envoyer un liquide du séparateur de phases à la colonne d'épuisement, une conduite pour soutirer un gaz enrichi en hydrogène de la colonne d'épuisement, une conduite pour soutirer un liquide appauvri en hydrogène de la colonne d'épuisement, des moyens pour diviser le liquide appauvri en hydrogène en une première portion et une deuxième portions, une conduite pour envoyer la première portion à l'état liquide dans la colonne de séparation CO/CH4, des moyens pour vaporiser la deuxième portion, des moyens pour envoyer la deuxième portion vaporisée à la colonne de séparation CO/CH4, une conduite pour soutirer un liquide riche en méthane de la colonne de séparation CO/CH4et une conduite pour soutirer un gaz riche en monoxyde de carbone de la colonne de séparation CO/CH4.An object of the present invention is to reduce the energy consumption of known solutions. Another object of the present invention is the reduction of temperature differences in at least one exchanger of the apparatus, in particular by reducing the maximum deviation, in at least one exchanger where liquids vaporize, to a value below 17 ° C or at 13 ° C. According to an object of the invention, there is provided a method of separation by cryogenic distillation of a mixture of hydrogen, carbon monoxide and methane and optionally nitrogen and / or argon and / or ethane wherein: i) the mixture is cooled and partially condensed ii) at least a portion of the formed liquid is fed to a depletion column to produce a hydrogen enriched overhead gas and a hydrogen depleted reactor liquid iii) the hydrogen-depleted liquid is divided into first and second portions, the first portion is sent in liquid form to a CO / CH4 separation column, the second portion is vaporized and sent in gaseous form to the separation column CO / CH4, iv) a high methane flow rate in the bottom of the CO / CH4 separation column and a carbon monoxide rich flow from the top of the CO / CH4 separation column are withdrawn. According to other optional aspects: the second portion is vaporized at at least two different pressures, after dividing it into at least two fractions. the different pressures are between the pressure of the depletion column and the pressure of the CO / CH4 separation column. - The second portion is vaporized by heat exchange with the mixture which cools. - the maximum temperature difference in the heat exchanger where the mixture cools and vaporizes the second portion does not exceed 17 ° C or 13 ° C. According to another object of the invention, there is provided an apparatus for separation by cryogenic distillation of a mixture of hydrogen, carbon monoxide and methane and optionally nitrogen and / or argon and / or the ethane comprising a phase separator, a depletion column, a CO / CH4 separation column and optionally a denitrogenation column, a heat exchanger, a pipe for sending the mixture to cool in the heat exchanger where it partially condenses, a conduit for supplying the partially condensed mixture of the heat exchanger to the phase separator, a conduit for supplying liquid from the phase separator to the depletion column, a conduit for withdrawing a hydrogen enriched gas from the depletion column, a conduit for withdrawing a depleted hydrogen liquid from the depletion column, means for dividing the hydrogen depleted liquid into a first portion and a second portion; me, a pipe for sending the first portion in the liquid state in the CO / CH4 separation column, means for vaporizing the second portion, means for sending the second vaporized portion to the CO / CH4 separation column, a conducted to withdraw a methane-rich liquid from the CO / CH4 separation column and a line for withdrawing a carbon monoxide-rich gas from the CO / CH4 separation column.
Selon d'autres objets facultatifs de l'invention, l'appareil comprend : - des moyens pour modifier la pression d'une fraction de la deuxième portion en amont de la vaporisation afin que la deuxième portion se vaporise à deux pressions différentes. - une colonne de déazotation, la conduite pour soutirer un gaz riche en monoxyde de carbone étant reliée à la colonne de déazotation. Eventuellement : - les moyens pour vaporiser la deuxième portion sont constitués par l'échangeur de chaleur. - la conduite de liquide appauvri en hydrogène est reliée à la partie inférieure de la colonne d'épuisement ainsi qu'à l'échangeur de chaleur afin de refroidir celui-ci en amont de la division en la première et la deuxième portions. L'invention sera décrite de manière plus détaillée par rapport à la figure qui montre un appareil selon l'invention. Dans la Figure 1, un débit de gaz de synthèse 1 contenant comme composants 15 principaux de l'hydrogène, du monoxyde de carbone et du méthane et éventuellement comprenant au moins comme composant mineur de l'azote est séparé par distillation cryogénique. Le débit 1 est épuré en eau dans une unité d'épuration 3 et éventuellement refroidi (ou réchauffé) dans le refroidisseur (ou réchauffeur) 5 pour former un débit refroidi (ou réchauffé) 20 7. Ce débit 7 est refroidi dans l'échangeur de chaleur 9 et ensuite dans l'échangeur de chaleur 11 pour être partiellement condensé. Le débit partiellement condensé est envoyé à un séparateur de phases V qui produit un gaz enrichi en hydrogène 13 et un liquide 15 appauvri en hydrogène. Le liquide 15 est détendu dans une vanne 17 et puis envoyé dans une colonne d'épuisement K1 . Le gaz de tête 21 de la colonne K1 , enrichi en hydrogène par rapport au 25 liquide 15, est envoyé à un échangeur de chaleur 49 et ensuite à un échangeur de chaleur 9. Le liquide de cuve de la colonne K1 est sous-refroidi dans l'échangeur de chaleur 11 et ensuite envoyé à un diviseur 23 où il se divise en au moins deux parties (dans la figure, en deux parties).Une partie 29 de liquide sous-refroidi est envoyée directement à la colonne de séparation CO/CH4 K2. Le reste 27 est envoyé à un diviseur 25 où il est divisé en deux parties. 30 Une partie essentiellement à la pression de la cuve de la colonne K1 est envoyée à l'échangeur de chaleur 11 où elle se vaporise. Ensuite elle est détendue dans une vanne 37 à la pression d'entrée de la colonne K2. L'autre partie 31 est détendue dans une vanne 35 jusqu'à la pression d'entrée de la colonne K2 en amont de l'échangeur de chaleur 11 et ensuite se réchauffe dans l'échangeur de chaleur 11 où elle se vaporise à une pression de vaporisation plus basse que celle de la partie 33.According to other optional objects of the invention, the apparatus comprises: means for modifying the pressure of a fraction of the second portion upstream of the vaporization so that the second portion vaporizes at two different pressures. a denitrogenization column, the pipe for withdrawing a gas rich in carbon monoxide being connected to the denitrogenation column. Optionally: the means for vaporizing the second portion consist of the heat exchanger. the hydrogen-depleted liquid line is connected to the lower part of the depletion column and to the heat exchanger in order to cool the latter upstream of the division into the first and the second portions. The invention will be described in more detail with respect to the figure which shows an apparatus according to the invention. In Figure 1, a synthesis gas flow 1 containing as major components hydrogen, carbon monoxide and methane and optionally comprising at least minor component of the nitrogen is separated by cryogenic distillation. The flow 1 is purified with water in a purification unit 3 and optionally cooled (or reheated) in the cooler (or heater) 5 to form a cooled (or heated) flow rate 7. This flow rate 7 is cooled in the exchanger 9 and then in the heat exchanger 11 to be partially condensed. The partially condensed flow is fed to a V phase separator which produces a hydrogen-enriched gas 13 and a hydrogen-depleted liquid. The liquid 15 is expanded in a valve 17 and then sent to a depletion column K1. The overhead gas 21 of the column K1, enriched in hydrogen with respect to the liquid 15, is sent to a heat exchanger 49 and then to a heat exchanger 9. The bottom liquid of the column K1 is subcooled in the heat exchanger 11 and then sent to a divider 23 where it is divided into at least two parts (in the figure, in two parts) .A portion 29 of subcooled liquid is sent directly to the separation column CO / CH4 K2. The remainder 27 is sent to a divider 25 where it is divided into two parts. A portion substantially at the pressure of the tank of the column K1 is sent to the heat exchanger 11 where it vaporizes. Then it is expanded in a valve 37 at the inlet pressure of the column K2. The other part 31 is expanded in a valve 35 to the inlet pressure of the column K2 upstream of the heat exchanger 11 and then heats up in the heat exchanger 11 where it vaporizes at a pressure vaporization rate lower than that of Part 33.
Les deux parties détendues et vaporisées sont réunies pour former le débit 39 qui alimente la colonne K2. Le liquide de cuve 41 de la colonne K2 riche en méthane se vaporise dans l'échangeur de chaleur 9. Le gaz de tête 43 de la colonne K2 enrichi en monoxyde de carbone est envoyé à la colonne de déazotation K3. La colonne K3 sert à séparer l'azote du monoxyde de carbone pour produire un liquide riche en monoxyde de carbone 45 en cuve de la colonne et un gaz 51 enrichi en azote et appauvri en monoxyde de carbone 51 en tête de colonne. La colonne K3 comprend un condenseur de tête 47 où se vaporise le liquide de cuve 45 avant d'être refroidi dans les échangeurs de chaleur 49 et 9. L'équilibre thermique de l'échangeur 11 est assuré également par la vaporisation de monoxyde de carbone liquide à une pression de vaporisation située entre 1.6 et 3 bar absolus.The two parts are expanded and vaporized together to form the flow 39 which feeds the column K2. The tank liquid 41 of the methane rich column K2 vaporizes in the heat exchanger 9. The overhead gas 43 of the carbon monoxide enriched column K2 is sent to the denitrogenation column K3. Column K3 serves to separate the nitrogen from the carbon monoxide to produce a carbon monoxide rich liquid 45 in the bottom of the column and a nitrogen-enriched 51 gas depleted of carbon monoxide 51 at the top of the column. Column K3 comprises a head condenser 47 where the tank liquid 45 vaporizes before being cooled in heat exchangers 49 and 9. The thermal equilibrium of exchanger 11 is also ensured by the vaporization of carbon monoxide liquid at a vaporization pressure between 1.6 and 3 bar absolute.
La présence de la colonne K3 est optionnelle, si le mélange 1 ne contient pas d'azote.The presence of column K3 is optional, if mixture 1 does not contain nitrogen.
Claims (10)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR1359525A FR3011320A1 (en) | 2013-10-02 | 2013-10-02 | METHOD AND APPARATUS FOR SEPARATION BY CRYOGENIC DISTILLATION OF A MIXTURE COMPRISING HYDROGEN, CARBON MONOXIDE AND METHANE |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR1359525A FR3011320A1 (en) | 2013-10-02 | 2013-10-02 | METHOD AND APPARATUS FOR SEPARATION BY CRYOGENIC DISTILLATION OF A MIXTURE COMPRISING HYDROGEN, CARBON MONOXIDE AND METHANE |
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| Publication Number | Publication Date |
|---|---|
| FR3011320A1 true FR3011320A1 (en) | 2015-04-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| FR1359525A Withdrawn FR3011320A1 (en) | 2013-10-02 | 2013-10-02 | METHOD AND APPARATUS FOR SEPARATION BY CRYOGENIC DISTILLATION OF A MIXTURE COMPRISING HYDROGEN, CARBON MONOXIDE AND METHANE |
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| FR (1) | FR3011320A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3599438A1 (en) | 2018-07-25 | 2020-01-29 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method and device for cryogenic separation of a mixture of carbon monoxide, hydrogen and methane for the production of ch4 |
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| EP0465366A1 (en) * | 1990-07-04 | 1992-01-08 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Process and installation for the simultaneous production of methane and carbon monoxide |
| DE4325513A1 (en) * | 1993-06-17 | 1994-12-22 | Linde Ag | Process for producing a highly pure carbon monoxide product stream and a hydrogen product stream |
| US6266976B1 (en) * | 2000-06-26 | 2001-07-31 | Air Products And Chemicals, Inc. | Cryogenic H2 and carbon monoxide production with an impure carbon monoxide expander |
| WO2008087318A2 (en) * | 2006-12-21 | 2008-07-24 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method for separating a mixture of carbon monoxide, methane, hydrogen, and optionally nitrogen by cryogenic distillation |
| FR2942869A1 (en) * | 2009-03-06 | 2010-09-10 | Air Liquide | Cryogenic separation method for mixture of carbon monoxide, hydrogen and nitrogen, involves constituting nitrogenless flow with final product at range or pressure higher than range set during pressurization in pump or compressor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0465366A1 (en) * | 1990-07-04 | 1992-01-08 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Process and installation for the simultaneous production of methane and carbon monoxide |
| DE4325513A1 (en) * | 1993-06-17 | 1994-12-22 | Linde Ag | Process for producing a highly pure carbon monoxide product stream and a hydrogen product stream |
| US6266976B1 (en) * | 2000-06-26 | 2001-07-31 | Air Products And Chemicals, Inc. | Cryogenic H2 and carbon monoxide production with an impure carbon monoxide expander |
| WO2008087318A2 (en) * | 2006-12-21 | 2008-07-24 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method for separating a mixture of carbon monoxide, methane, hydrogen, and optionally nitrogen by cryogenic distillation |
| FR2942869A1 (en) * | 2009-03-06 | 2010-09-10 | Air Liquide | Cryogenic separation method for mixture of carbon monoxide, hydrogen and nitrogen, involves constituting nitrogenless flow with final product at range or pressure higher than range set during pressurization in pump or compressor |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3599438A1 (en) | 2018-07-25 | 2020-01-29 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method and device for cryogenic separation of a mixture of carbon monoxide, hydrogen and methane for the production of ch4 |
| US20200033055A1 (en) * | 2018-07-25 | 2020-01-30 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Process and apparatus for the cryogenic separation of a mixture of carbon monoxide, hydrogen and methane for the production of ch4 |
| FR3084453A1 (en) * | 2018-07-25 | 2020-01-31 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | PROCESS AND APPARATUS FOR CRYOGENIC SEPARATION OF A MIXTURE OF CARBON MONOXIDE, HYDROGEN AND METHANE FOR THE PRODUCTION OF CH4 |
| US11965694B2 (en) | 2018-07-25 | 2024-04-23 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Process and apparatus for the cryogenic separation of a mixture of carbon monoxide, hydrogen and methane for the production of CH4 |
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