EP2504646B1 - Method and apparatus for cryogenically separating a mixture of nitrogen and carbon monoxide - Google Patents
Method and apparatus for cryogenically separating a mixture of nitrogen and carbon monoxide Download PDFInfo
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- EP2504646B1 EP2504646B1 EP10792965.5A EP10792965A EP2504646B1 EP 2504646 B1 EP2504646 B1 EP 2504646B1 EP 10792965 A EP10792965 A EP 10792965A EP 2504646 B1 EP2504646 B1 EP 2504646B1
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- carbon monoxide
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- phase separator
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims description 47
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims description 36
- 229910002091 carbon monoxide Inorganic materials 0.000 title claims description 36
- 238000000034 method Methods 0.000 title claims description 11
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims description 8
- 239000000203 mixture Substances 0.000 title description 4
- 239000007789 gas Substances 0.000 claims description 55
- 239000007788 liquid Substances 0.000 claims description 49
- 238000004519 manufacturing process Methods 0.000 claims description 23
- 238000004821 distillation Methods 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 17
- 238000000926 separation method Methods 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000003245 coal Substances 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000005201 scrubbing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000000629 steam reforming Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241001415961 Gaviidae Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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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
- F25J2200/40—Features relating to the provision of boil-up in the bottom of a column
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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
- F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead 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
- 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
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/42—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
- F25J2270/00—Refrigeration techniques used
- F25J2270/02—Internal refrigeration with liquid vaporising loop
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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
- F25J2270/04—Internal refrigeration with work-producing gas expansion loop
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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
- F25J2270/24—Quasi-closed internal or closed external carbon monoxide refrigeration cycle
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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
- F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
- F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop
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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
- F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
- F25J2290/34—Details about subcooling of liquids
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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
- F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
- F25J2290/80—Retrofitting, revamping or debottlenecking of existing plant
Definitions
- the present invention relates to a method and apparatus for cryogenic separation of a mixture of nitrogen and carbon monoxide, according to the preambles of claims 1 and 4 respectively and known from the document DE-A-2,147,465 .
- the most common cryogenic process is methane scrubbing
- the residual methane content in the synthesis gas is compatible with the methane washing process.
- a methane scrubbing scheme with a CO / N 2 column is described in FR-A-2910603 .
- the synthesis gas produced is treated in a cold box by partial condensation without a cycle, the inert content (CH 4 , Ar and N 2 ) being very low and compatible with the purity of the product. CO.
- a partial condensation scheme with a CO / N 2 column is described in US-A-4478621 .
- the reboiling of the column CO / N 2 is provided by a direct supply of CO at medium pressure in the bottom of the column coming from the compressor CO.
- the apparatus according to the invention is a partial condensation apparatus including a CO / N 2 column with a common integrated cycle for the cooling of the synthesis gas and for the separation energy CO / N 2 .
- At least a portion of the reboiling energy of the CO / N 2 column is provided by an external reboiler where the feed gas of the CO / N 2 column is condensed totally or partially. This makes it possible to reduce the MPCO flow rate of the cycle compressor and thus reduce the energy of the compressor by about 15%.
- the process scheme may include a CO / N 2 distillation column alone or a CO / N 2 column with a CO / CH 4 column.
- This invention can also be applied when it is desired to invest a CO / N 2 separation column treating impure CO coming from a cold box which does not comprise a CO / N 2 column. As the nitrogen content in CO increases over time, it then becomes necessary to add a CO / N 2 separation step. The new column is then installed in a dedicated cold box that must be supplied with frigories and reboiling energy.
- DE-A-4228784 and DE-A-2147465 describe processes comprising the features of the preamble of claim 1 and similar to that of Figure 1 .
- a flow of nitrogen and carbon monoxide 1 is cooled in an exchanger 3. It is condensed at least partially in a reboiler 5 fed by the liquid column of the column 15. The vaporized liquid is returned to the column.
- the at least partially condensed flow rate is expanded in a valve 7 and sent to a phase separator 9. the liquid 11 of the phase separator and the gas 13 of the phase separator 9 are sent to the column at different heights or not.
- the bottom liquid of the column is expanded in a valve 19 and sent to the head condenser 23 forming part of the column.
- a nitrogen flow is removed as a purge and heats up in the exchanger 3.
- the vaporized carbon monoxide 27 also heats up in the exchanger 3 and is compressed in the first stage 29 of a compressor. It is cooled in a cooler 31 by water and then divided in two. The flow 33 cools to an intermediate temperature in the exchanger 3 to form the flow 45 which is sent to the bottom of the column 15. The flow 41 is cooled very partially in the exchanger 3, expanded in a turbine 43 and The remainder of the carbon monoxide is compressed at the product pressure by the compressor stage 37 and cooled by the cooler 31A to form the product flow 39.
- the stage 29 is all the more small part of the reboil is provided by flow 1.
- a flow of nitrogen, hydrogen and carbon monoxide 1 is cooled in an exchanger 3 and then in a heat exchanger 3A.
- the flow 1 is sent to a first phase separator 51 where it separates into a flow rate 53 rich in hydrogen and a liquid flow 57.
- the flow 53 is heated in the exchangers 3,3A and the flow 57 is expanded in a valve 55 and then sent to a second phase separator 61.
- the gas of the second separator of phases is heated in the heat exchangers 3,3A to form the flow 77.
- the liquid 63 is separated in two.
- a portion 67 is expanded in a valve 69, sent to a phase separator 71 and then the flow rates 73,75 are sent to the distillation column 15.
- the remainder 65 of the liquid of the separator 61 is heated in the exchanger 3A to forming the flow 65 which serves to heat the reboiler 5 fed by the tank liquid 17 of the column 15. Having served to reboil the column, the flow 65 is expanded in the valve 7, sent to the separator 9 and then to the column of the same way as for the Figure 1 .
- a nitrogen flow is removed as a purge and heats up in the exchanger 3.
- the vaporized carbon monoxide 27 also heats up in the exchanger 3 and is compressed in the first stage 29 of a compressor. It is cooled in a cooler 31 by water and then divided in two.
- the flow 33 cools to an intermediate temperature in the exchanger 3 and is divided in two to form the flow 133.
- This flow 133 is cooled in the exchanger 135 against liquid nitrogen 137.
- the liquid nitrogen 137 vaporizes and heats in the exchanger 3.
- the flow 133 is expanded and mixed with the flow 21 downstream of the valve 19.
- the flow 45 is sent to the bottom of the column 5 after cooling in the exchanger 3A.
- the liquid carbon monoxide 79 is withdrawn from the condenser 23, expanded in the valve 81, sent to the phase separator 83 to produce a liquid portion and a gas portion.
- the liquid portion 85 vaporizes in the exchange line 3A and the gas 87 is mixed with the flow rate of carbon monoxide 27 for the compressor 29.
- a flow of nitrogen, hydrogen and carbon monoxide 1 is cooled in an exchanger 3 and then in a heat exchanger 3A.
- the flow 1 is sent to a first phase separator 51 where it separates into a gaseous flow 53 rich in hydrogen and a liquid flow 57.
- the flow 53 is heated in the exchangers 3,3A and the flow 57 is expanded in a valve 55 and then sent to a second phase separator 61.
- the gas of the second phase separator heats up in the exchangers 3,3A to form the flow 77.
- the liquid 63 is separated in two.
- a portion 67 is expanded in a valve 69, sent to a phase separator 71 and then the flow rates 73,75 are sent to the distillation column 5.
- the remainder 65 of the liquid of the separator 61 is heated in the exchanger 3A to forming the flow 65 which serves to heat the reboiler 5 fed by the tank liquid 17 of the column 5. Having served to reboil the column the flow 65 is expanded in the valve 7, sent to the separator 9 and then to the column of the same way as for the Figure 1 .
- a nitrogen flow is removed as a purge and is heated in the exchanger 3.
- the vaporized carbon monoxide enriched flow 27 also warms up in the exchanger 3 and is compressed in the first stage 29 of a compressor. It is cooled in a cooler 31 by water and then divided in two.
- the flow 33 cools to an intermediate temperature in the exchanger 3 and is divided in two to form the flow 93.
- This flow 93 is expanded in the turbine 91 to form the expanded flow 93 which is mixed with the flow 27 for to heat up in the exchanger 3.
- the flow 45 from the stage 29 is sent to the bottom of the column 5 after cooling in the exchanger 3A.
- the liquid carbon monoxide 79 is withdrawn from the condenser 23, expanded in the valve 81, sent to the phase separator 83 to produce a liquid portion and a gas portion.
- the liquid portion 85 vaporizes in the exchange line 3A and the gas 87 is mixed with the flow rate of carbon monoxide 27 for the compressor 29.
Description
La présente invention est relative à un procédé et à un appareil de séparation cryogénique d'un mélange d'azote et de monoxyde de carbone, conformément aux préambules des revendications 1 et 4 respectivement et connu du document
Les unités de production de monoxyde de carbone et d'hydrogène peuvent être séparées en deux parties :
- génération du gaz de synthèse (mélange contenant H2, CO, CH4, CO2, Ar et N2 essentiellement). Parmi les diverses voies industrielles de production de gaz de synthèse, celle à base de gazéification de charbon semble se développer de plus en plus notamment dans les pays riches en dépôts de charbon comme la Chine. Le procédé d'oxydation partielle du gaz naturel peut s'avérer également intéressant pour la production de CO seul ou avec des rapports de production H2/CO faible. Une autre voie est le reformage à la vapeur.
- purification du gaz de synthèse. On retrouve :
- une unité de lavage avec un solvant liquide pour éliminer la plus grande partie des gaz acides contenus dans le gaz de synthèse
- une unité d'épuration sur lit d'adsorbants.
- une unité de séparation par voie cryogénique dite boite froide pour la production de CO.
- generation of the synthesis gas (mixture containing H 2 , CO, CH 4 , CO 2 , Ar and N 2 essentially). Among the various synthetic gas production industries, the one based on coal gasification seems to develop more and more particularly in countries rich in coal deposits such as China. The partial oxidation process of natural gas can also be interesting for the production of CO alone or with low H 2 / CO production ratios. Another way is steam reforming.
- purification of the synthesis gas . We find :
- a washing unit with a liquid solvent to remove most of the acid gases contained in the synthesis gas
- an adsorbent bed purification unit.
- cryogenic separation unit called cold box for the production of CO.
Dans le cas d'un gaz de synthèse issu d'un four de reformage à la vapeur, pour la production de CO et d'hydrogène sous pression, le procédé cryogénique le plus fréquent est le lavage au méthane, la teneur résiduelle en méthane dans le gaz de synthèse étant compatible avec le procédé lavage au méthane. Dans certains cas il est nécessaire d'inclure une colonne de séparation CO/N2 dans la boite froide notamment quand la teneur en azote dans le gaz naturel n'est pas compatible avec la pureté du produit CO sans cette colonne CO/N2.In the case of synthesis gas from a steam reforming furnace, for the production of CO and hydrogen under pressure, the most common cryogenic process is methane scrubbing, the residual methane content in the synthesis gas is compatible with the methane washing process. In some cases it is necessary to include a CO / N 2 separation column in the cold box, especially when the nitrogen content in the natural gas is not compatible with the purity of the CO product without this CO / N 2 column.
Un schéma lavage au méthane avec colonne CO/N2 est décrit dans
Dans le cas de certains procédé de gazéification de charbon, le gaz de synthèse produit est traité dans une boite froide par condensation partielle sans cycle, la teneur en inertes (CH4, Ar et N2) étant très faible et compatible avec la pureté du CO.In the case of some coal gasification process, the synthesis gas produced is treated in a cold box by partial condensation without a cycle, the inert content (CH 4 , Ar and N 2 ) being very low and compatible with the purity of the product. CO.
Un schéma condensation partielle sans colonne de séparation est décrit dans
Un schéma de condensation partielle avec une colonne CO/N2 est décrit dans
Dans le cas où la teneur en méthane dans le gaz de synthèse ne permet pas un procédé de lavage au méthane dans la production combinée de CO et d'hydrogène et où la teneur en azote dans le gaz de synthèse n'est pas compatible avec la pureté de CO sans séparation CO/N2, l'appareil selon l'invention est un appareil de condensation partielle incluant une colonne CO/N2 avec cycle intégré commun pour le refroidissement du gaz de synthèse et pour l'énergie de séparation CO/N2.In the case where the methane content in the synthesis gas does not allow a methane scrubbing process in the combined production of CO and hydrogen and where the nitrogen content in the synthesis gas is not compatible with the CO purity without CO / N 2 separation, the apparatus according to the invention is a partial condensation apparatus including a CO / N 2 column with a common integrated cycle for the cooling of the synthesis gas and for the separation energy CO / N 2 .
Au moins une partie de l'énergie de rebouillage de la colonne CO/N2 est apportée par un rebouilleur externe où le gaz d'alimentation de la colonne CO/N2 est condensé totalement ou partiellement. Cela permet de réduire le débit MPCO du compresseur de cycle et ainsi réduire l'énergie du compresseur de l'ordre de 15%.At least a portion of the reboiling energy of the CO / N 2 column is provided by an external reboiler where the feed gas of the CO / N 2 column is condensed totally or partially. This makes it possible to reduce the MPCO flow rate of the cycle compressor and thus reduce the energy of the compressor by about 15%.
Le schéma de procédé peut inclure une colonne de distillation CO/N2 seule ou bien une colonne CO/N2 avec une colonne CO/CH4.The process scheme may include a CO / N 2 distillation column alone or a CO / N 2 column with a CO / CH 4 column.
Cette invention peut s'appliquer également lorsque l'on souhaite investir une colonne de séparation CO/N2 traitant du CO impur venant d'une boite froide qui ne comprend pas de colonne CO/N2. La teneur d'azote dans le CO augmentant dans le temps, il devient alors nécessaire de rajouter une étape de séparation CO/N2. La nouvelle colonne est alors installée dans une boite froide dédiée qu'il faut alimenter en frigories et en énergie de rebouillage.This invention can also be applied when it is desired to invest a CO / N 2 separation column treating impure CO coming from a cold box which does not comprise a CO / N 2 column. As the nitrogen content in CO increases over time, it then becomes necessary to add a CO / N 2 separation step. The new column is then installed in a dedicated cold box that must be supplied with frigories and reboiling energy.
Selon un objet de l'invention, il est prévu un procédé de séparation d'un gaz d'alimentation contenant comme composants principaux de l'azote et du monoxyde de carbone et éventuellement de l'hydrogène dans une colonne de distillation dans lequel :
- i) on refroidit le gaz d'alimentation dans un échangeur de chaleur (3)
- ii) on envoie au moins une partie d'un gaz dérivé du gaz d'alimentation à un rebouilleur de cuve de la colonne de distillation afin de la condenser au moins partiellement en produisant un liquide et éventuellement un gaz
- iii) on envoie au moins une partie du liquide et éventuellement au moins une partie du gaz à la colonne
- iv) on soutire un débit enrichi en azote gazeux de la colonne
- v) on soutire un débit enrichi en monoxyde de carbone de la colonne, on le réchauffe dans l'échangeur de chaleur caractérisé en ce que l'on comprime le débit enrichi en monoxyde de carbone pour fournir un produit enrichi en monoxyde de carbone à une pression de production, on envoie le gaz d'alimentation après refroidissement dans un premier séparateur de phases, on détend le liquide du premier séparateur de phases , on envoie le liquide détendu dans un deuxième séparateur de phases et on vaporise au moins une partie du liquide du deuxième séparateur de phases pour dériver le gaz à envoyer au rebouilleur.
- i) the feed gas is cooled in a heat exchanger (3)
- ii) at least a portion of a gas derived from the feed gas is sent to a bottom reboiler of the distillation column in order to condense it at least partially by producing a liquid and optionally a gas
- iii) at least a portion of the liquid and at least a portion of the gas is sent to the column
- iv) a flow enriched in nitrogen gas from the column is withdrawn
- v) a carbon monoxide enriched flow is withdrawn from the column, it is heated in the heat exchanger characterized in that the carbon monoxide enriched flow is compressed to provide a product enriched in carbon monoxide at a rate of production pressure, the feed gas is sent after cooling in a first phase separator, the liquid is depressurized from the first phase separator, the expanded liquid is sent to a second phase separator and at least a portion of the liquid is vaporized the second phase separator for diverting the gas to be sent to the reboiler.
Eventuellement :
- on comprime une partie du monoxyde de carbone à une pression inférieure ou égale à la pression de production, on la refroidit dans l'échangeur de chaleur et on l'envoie en cuve de la colonne de distillation.
- on vaporise l'au moins une partie du liquide du deuxième séparateur de phases dans l'échangeur de chaleur.
- a portion of the carbon monoxide is compressed at a pressure less than or equal to the production pressure, cooled in the heat exchanger and sent to the bottom of the distillation column.
- the at least a portion of the liquid of the second phase separator is vaporized in the heat exchanger.
Selon un autre aspect de l'invention, il est prévu un appareil de séparation d'un gaz d'alimentation contenant comme composants principaux de l'azote et du monoxyde de carbone et éventuellement de l'hydrogène comprenant :
- i) une colonne de distillation ayant un rebouilleur de cuve et éventuellement un condenseur de tête
- ii) un échangeur de chaleur
- iii) un compresseur
- iv) des moyens pour envoyer le gaz d'alimentation dans l'échangeur de chaleur
- v) des moyens pour envoyer au moins une partie d'un gaz dérivé du gaz d'alimentation au rebouilleur afin de la condenser au moins partiellement en produisant un liquide et éventuellement un gaz
- vi) au moins des moyens pour envoyer au moins une partie du liquide et éventuellement au moins une partie du gaz à la colonne
- vii) des moyens pour soutirer un débit enrichi en azote gazeux de la colonne
- viii)des moyens pour soutirer un débit enrichi en monoxyde de carbone de la colonne et pour l'envoyer à l'échangeur de chaleur caractérisé en ce qu'il comprend des moyens pour envoyer le débit enrichi en monoxyde de carbone au compresseur pour fournir un produit enrichi en monoxyde de carbone à une pression de production, un premier séparateur de phases (51), un deuxième séparateur de phases, des moyens pour envoyer le gaz d'alimentation refroidi dans le premier séparateur de phases, une vanne de détente pour détendre le liquide du premier séparateur de phases, des moyens pour envoyer le liquide détendu dans le deuxième séparateur de phases et des moyens pour vaporiser au moins une partie du liquide du deuxième séparateur de phases pour dériver le gaz à envoyer au rebouilleur .
- i) a distillation column having a bottom reboiler and optionally a top condenser
- ii) a heat exchanger
- iii) a compressor
- iv) means for sending the feed gas into the heat exchanger
- v) means for sending at least a portion of a gas derived from the feed gas to the reboiler in order to condense it at least partially by producing a liquid and optionally a gas
- vi) at least means for sending at least a portion of the liquid and optionally at least a portion of the gas to the column
- vii) means for withdrawing a flow enriched in gaseous nitrogen from the column
- viii) means for withdrawing a carbon monoxide enriched flow from the column and for sending it to the heat exchanger, characterized in that it comprises means for sending the flow enriched in carbon monoxide to the compressor to provide a product enriched in carbon monoxide at a production pressure, a first phase separator (51), a second phase separator, means for sending the cooled feed gas into the first phase separator, an expansion valve to relax the liquid of the first phase separator, means for sending the expanded liquid to the second phase separator and means for vaporizing at least a portion of the liquid of the second phase separator to divert the gas to be sent to the reboiler.
Optionnellement, l'appareil comprend :
- des moyens pour envoyer une partie du débit enrichi en monoxyde de carbone à une pression inférieure ou égale à la pression de production à l'échangeur de chaleur et ensuite en cuve de la colonne de distillation .
- l'échangeur de chaleur est relié à la colonne et au deuxième séparateur de phases afin de vaporiser au moins une partie du liquide du deuxième séparateur pour dériver le gaz de chauffage du rebouilleur de cuve
- la colonne de distillation comprend un condenseur de tête.
- des moyens pour envoyer le liquide de cuve de la colonne au condenseur de tête.
- des moyens pour envoyer le liquide de cuve vaporisé au compresseur.
- means for sending a portion of the carbon monoxide enriched flow at a pressure less than or equal to the production pressure to the heat exchanger and then in the distillation column.
- the heat exchanger is connected to the column and the second phase separator to vaporize at least a portion of the liquid of the second separator to divert the heating gas from the reboiler
- the distillation column comprises a top condenser.
- means for sending the tank liquid from the column to the overhead condenser.
- means for sending the vaporized tank liquid to the compressor.
L'invention sera décrite en plus de détails en se référant aux figures qui représentent un appareil de séparation substantiellement selon l'art antérieur d'un gaz ayant comme composants principaux de l'azote et du monoxyde de carbone pour la
Selon la
Selon la
Un débit d'azote est enlevé comme purge 25 et se réchauffe dans l'échangeur 3. Le monoxyde de carbone vaporisé 27 se réchauffe également dans l'échangeur 3 et est comprimé dans la première étage 29 d'un compresseur. Il est refroidi dans un refroidisseur 31 par de l'eau et ensuite divisé en deux. Le débit 33 se refroidit jusqu'à une température intermédiaire dans l'échangeur 3 et est divisé en deux pour former le débit 133. Ce débit 133 se refroidit dans l'échangeur 135 contre de l'azote liquide 137. L'azote liquide 137 se vaporise et se réchauffe dans l'échangeur 3. Le débit 133 est détendu et mélangé avec le débit 21 en aval de la vanne 19. Le débit 45 est envoyé en cuve de la colonne 5 après refroidissement dans l'échangeur 3A.A nitrogen flow is removed as a purge and heats up in the
Le monoxyde de carbone liquide 79 est soutiré du condenseur 23, détendu dans la vanne 81, envoyé au séparateur de phases 83 pour produire une partie liquide et une partie gazeuse. La partie liquide 85 se vaporise dans la ligne d'échange 3A et le gaz 87 est mélangé au débit de monoxyde de carbone 27 destiné au compresseur 29.The
Selon la
Un débit d'azote est enlevé comme purge 25 et se réchauffe dans l'échangeur 3. Le débit enrichi en monoxyde de carbone vaporisé 27 se réchauffe également dans l'échangeur 3 et est comprimé dans la première étage 29 d'un compresseur. Il est refroidi dans un refroidisseur 31 par de l'eau et ensuite divisé en deux. Le débit 33 se refroidit jusqu'à une température intermédiaire dans l'échangeur 3 et est divisé en deux pour former le débit 93. Ce débit 93 se détendu dans la turbine 91 pour former le débit détendu 93 qui est mélangé avec le débit 27 pour se réchauffer dans l'échangeur 3. Le débit 45 provenant de l'étage 29 est envoyé en cuve de la colonne 5 après refroidissement dans l'échangeur 3A.A nitrogen flow is removed as a purge and is heated in the
Le monoxyde de carbone liquide 79 est soutiré du condenseur 23, détendu dans la vanne 81, envoyé au séparateur de phases 83 pour produire une partie liquide et une partie gazeuse. La partie liquide 85 se vaporise dans la ligne d'échange 3A et le gaz 87 est mélangé au débit de monoxyde de carbone 27 destiné au compresseur 29.The
Claims (9)
- Method for separating a feed gas containing, as the main components, nitrogen and carbon monoxide and optionally hydrogen in a distillation column (15) wherein:i) the feed gas is cooled in a heat exchanger (3)ii) at least part of a gas derived from the feed gas is sent to a vessel reboiler (5) of the distillation column in order to at least partially condense it, producing a liquid and optionally a gasiii) at least part of the liquid and optionally at least part of the gas is sent to the columniv) a flow enriched with gaseous nitrogen is drawn off from the columnv) a flow enriched with carbon monoxide is drawn off from the column and is heated in the heat exchanger, characterised in that the flow enriched with carbon monoxide is compressed in order to supply a product enriched with carbon monoxide at a production pressure, the feed gas is sent after cooling into a first phase separator (51), the liquid from the first phase separator (61) is expanded, the expanded liquid is sent into a second phase separator and at least part of the liquid from the second phase separator is vaporised in order to derive the gas to be sent to the vessel reboiler.
- Method according to claim 1, wherein part of the carbon monoxide is compressed at a pressure less than or equal to the production pressure, is cooled in the heat exchanger (3) and is sent to the vessel of the distillation column (15).
- Method according to claim 1, wherein at least part of the liquid from the second phase separator (61) is vaporised in the heat exchanger (33).
- Apparatus for separating a feed gas containing, as the main components, nitrogen and carbon monoxide and optionally hydrogen, comprising:a. a distillation column (15) having a vessel reboiler (5) and optionally a head condenser (23)b. a heat exchanger (3)c. a compressor (29, 37)d. means for sending the feed gas into the heat exchangere. means for sending at least part of a gas derived from the feed gas to the reboiler in order to at least partially condense it, producing a liquid and optionally a gasf. at least means for sending at least part of the liquid and optionally at least part of the gas to the columng. means for drawing off a flow enriched with gaseous nitrogen from the columnh. means for drawing off a flow enriched with carbon monoxide from the column and sending it to the heat exchanger, characterised in that it comprises means for sending the flow enriched with carbon monoxide to the compressor in order to supply a product enriched with carbon monoxide at a production pressure, a first phase separator (51), a second phase separator (61), means for sending the cooled feed gas into the first phase separator, an expansion valve (55) for expanding the liquid from the first phase separator, means for sending the expanded liquid into the second phase separator and means (3) for vaporising at least part of the liquid from the second phase separator in order to derive the gas to be sent to the vessel reboiler (5).
- Apparatus according to claim 4, comprising means for sending part of the flow enriched with carbon monoxide at a pressure less than or equal to the production pressure to the heat exchanger (3) and next to the vessel of the distillation column (15).
- Apparatus according to claim 4, wherein the heat exchanger (3) is connected to the column (15) and to the second phase separator (61) in order to vaporise at least part of the liquid from the second separator in order to derive the heating gas for the vessel reboiler (5).
- Apparatus according to claim 4, wherein the distillation column comprises a head condenser.
- Apparatus according to claim 7, comprising means for sending the vessel liquid from the column to the head condenser.
- Apparatus according to claim 8, comprising means for sending the vaporised vessel liquid to the compressor.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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FR0958305A FR2953004B1 (en) | 2009-11-24 | 2009-11-24 | PROCESS FOR CRYOGENIC SEPARATION OF A NITROGEN MIXTURE AND CARBON MONOXIDE |
PCT/FR2010/052368 WO2011067492A2 (en) | 2009-11-24 | 2010-11-04 | Method for cryogenically separating a mixture of nitrogen and carbon monoxide |
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EP2504646B1 true EP2504646B1 (en) | 2019-01-02 |
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EP10792965.5A Active EP2504646B1 (en) | 2009-11-24 | 2010-11-04 | Method and apparatus for cryogenically separating a mixture of nitrogen and carbon monoxide |
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US (1) | US9625209B2 (en) |
EP (1) | EP2504646B1 (en) |
JP (1) | JP2013511697A (en) |
CN (1) | CN102893110B (en) |
FR (1) | FR2953004B1 (en) |
WO (1) | WO2011067492A2 (en) |
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FR2982168B1 (en) * | 2011-11-04 | 2015-05-01 | Air Liquide | PROCESS AND APPARATUS FOR SEPARATING CARBON DIOXIDE-RICH GAS BY DISTILLATION |
FR3011069B1 (en) * | 2013-09-24 | 2015-09-11 | Air Liquide | METHOD AND APPARATUS FOR CRYOGENIC SEPARATION OF A MIXTURE CONTAINING AT LEAST CARBON MONOXIDE, HYDROGEN AND NITROGEN |
FR3013107A1 (en) * | 2013-11-14 | 2015-05-15 | Air Liquide | METHOD AND APPARATUS FOR DEAZATING A FLUID RICH IN CARBON MONOXIDE |
FR3084453B1 (en) * | 2018-07-25 | 2020-11-27 | Air Liquide | METHOD AND APPARATUS FOR THE CRYOGENIC SEPARATION OF A MIXTURE OF CARBON MONOXIDE, HYDROGEN AND METHANE FOR THE PRODUCTION OF CH4 |
DE102020130946B4 (en) * | 2020-11-23 | 2023-02-02 | Xenon Holding Gmbh | Cryogenic process for recovering valuable substances from a hydrogen-rich feed gas |
FR3118144A3 (en) * | 2020-12-22 | 2022-06-24 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | METHOD AND APPARATUS FOR THE CRYOGENIC SEPARATION OF A MIXTURE OF HYDROGEN, METHANE, NITROGEN AND CARBON MONOXIDE |
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DE3822175A1 (en) * | 1988-06-30 | 1990-01-04 | Linde Ag | Process for removing nitrogen from nitrogen-containing natural gas |
FR2664263B1 (en) * | 1990-07-04 | 1992-09-18 | Air Liquide | PROCESS AND PLANT FOR THE SIMULTANEOUS PRODUCTION OF METHANE AND CARBON MONOXIDE. |
DE4210637A1 (en) * | 1992-03-31 | 1993-10-07 | Linde Ag | Process for the production of high-purity hydrogen and high-purity carbon monoxide |
DE4228784A1 (en) * | 1992-08-28 | 1994-03-03 | Linde Ag | Process to separate constituents of a gas mixt. with a single-stage rectifier at low temp. - needs no expansion chamber or compressor |
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- 2010-11-04 WO PCT/FR2010/052368 patent/WO2011067492A2/en active Application Filing
- 2010-11-04 JP JP2012540471A patent/JP2013511697A/en not_active Withdrawn
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FR2953004B1 (en) | 2013-12-20 |
FR2953004A1 (en) | 2011-05-27 |
CN102893110A (en) | 2013-01-23 |
CN102893110B (en) | 2014-11-26 |
US20120279254A1 (en) | 2012-11-08 |
US9625209B2 (en) | 2017-04-18 |
JP2013511697A (en) | 2013-04-04 |
WO2011067492A2 (en) | 2011-06-09 |
WO2011067492A3 (en) | 2014-03-20 |
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