Classifications

• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
  • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
  • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
  • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
  • F25J3/0204—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
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
  • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
  • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
  • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
  • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
  • F25J3/0252—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of hydrogen
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
  • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
  • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
  • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
  • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
  • F25J3/0257—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of nitrogen
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
  • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
  • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
  • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
  • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
  • F25J3/0261—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of carbon monoxide
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
  • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
  • 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
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
  • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
  • F25J2200/00—Processes or apparatus using separation by rectification
  • F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead gas
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
  • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
  • F25J2205/00—Processes or apparatus using other separation and/or other processing means
  • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
• • 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
• • 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
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
  • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
  • F25J2270/00—Refrigeration techniques used
  • F25J2270/04—Internal refrigeration with work-producing gas expansion loop
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
  • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
  • F25J2270/00—Refrigeration techniques used
  • F25J2270/24—Quasi-closed internal or closed external carbon monoxide refrigeration cycle
• • 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
  • F25J2280/00—Control of the process or apparatus
  • F25J2280/02—Control in general, load changes, different modes ("runs"), measurements

Definitions

• the present invention relates to a process for separating a mixture of carbon monoxide, nitrogen, hydrogen and optionally methane by cryogenic distillation.
• denitrogenation column whose function is to produce carbon monoxide tank at the required purity.
• a nitrogen purge containing a fraction of CO is recovered.
• the denitrogenation column is located either upstream or downstream of the CO / CH 4 separation column.
• the reboiling of the denitrogenation column is provided by an injection of carbon monoxide in the form of steam in the bottom of the column.
• This carbon monoxide comes from several sources, one of which is the vaporization of liquid carbon monoxide at medium pressure in the exchange line.
• This carbon monoxide medium pressure is therefore high pressure carbon monoxide which has been liquefied and who will thus have two jobs:
• the average carbon dioxide vapor pressure flow rate will be dimensioned by the exchange line or by the maximum permissible fraction in the reboiling of the column CO / N 2 .
• the present invention aims to eliminate this constraint which leads to a significant energy loss on the current estimates, as well as to eliminate the output of medium pressure gas on the compressor which compresses the carbon monoxide up to the high pressure (line, filter, valves, passages in exchangers, regulations, etc.).
• a process for separating a mixture of carbon monoxide, nitrogen, hydrogen and optionally methane by cryogenic distillation in a separation means system comprising a turbine, a methane washing column, a depletion column, a CO / CH 4 column and a denitrogenation column, the denitrogenation column being downstream or upstream of the CO / CH 4 column in which the mixture is separated to obtain a carbon monoxide enriched fluid containing nitrogen, this fluid is separated in the denitrogenation column, a carbon monoxide flow rate from the column system in a compressor is compressed to a high pressure, optionally between 25 and 45 bar, high pressure carbon monoxide is sent from the compressor to the turbine and from the turbine to the denitrogenation column, a high pressure carbon monoxide flow fraction serves as a product and is cooled said another part of the carbon monoxide at high pressure, optionally between 25 and 45 bar, before the relaxation characterized in that at least one punctually relaxes a variable amount of
• the high pressure is between 25 and 45 bar; a flow rate of carbon monoxide-rich gas sent to the bottom of the denitrogenation column is measured, and the sending of high-pressure carbon monoxide expanded in the valve is triggered as a function of the flow of carbon monoxide-rich gas sent to the tank; the denitrogenation column; - the sending of high pressure carbon monoxide expanded in the valve is triggered if the flow rate of carbon monoxide gas sent to the denitrogenation column is reduced by at least 5% or even at least 10% relative to the flow rate nominal; the high pressure corresponds to the outlet pressure of the last stage of the compressor.
• a plant for separating a mixture of carbon monoxide, nitrogen, hydrogen and optionally methane by cryogenic distillation in a separation means system comprising a turbine, a methane washing column, a depletion column, a CO / CH 4 column and a denitrogenation column, the denitrogenation column being downstream or upstream of the CO / CH 4 column, means for sending the mixture to the system separation means for obtaining a carbon monoxide-enriched fluid containing nitrogen, means for supplying said fluid into the denitrogenation column, a compressor, means for sending a carbon monoxide flow from the column system to the compressor and means for collecting a flow of carbon monoxide at a high pressure at the outlet of the compressor, means for sending a portion of the high pressure flow to the turbine and the tur a means for sending another portion of the high pressure stream to a bottom reboiler of the depletion column and / or the CO / CH 4 column; means for recovering a monoxide
• the installation comprises means for measuring a flow rate of carbon monoxide rich gas sent to the tank.
• the idea is to dimension the apparatus without the stress on the reboiling fraction independent of the vapor pressure medium carbon monoxide (and thus it is accepted that all the reboiling can come from the vaporization of the medium pressure carbon monoxide). Then a line is installed between the high-pressure carbon monoxide outlet to the reboilers of the exhaust column and the CO / CH 4 column (approximately -110 0 C) and the reboiling feed of the CO / N 2 column.
• This line will therefore lead to the investment of the line itself and of a single valve (there are already the valves on the upstream lines going to the reboilers fed by the high pressure carbon monoxide) and downstream (monoxide of medium vaporized pressure carbon)).
• the medium pressure carbon monoxide thus produced does not pass in a line of exchange and the flow can be set to zero for a running of the device. In operation, if it is desired to reduce the average vaporized pressure carbon monoxide while maintaining a higher reboil flow rate, it is sufficient to supplement this medium pressure carbon monoxide.
• This invention is generalizable to all methane washing apparatus with denitration in the current scheme.
• the flow rate of carbon monoxide medium pressure that can be vaporized in the exchange line is significantly lower than the reboiling rate, it will nonetheless be interesting to install a medium pressure outlet on the compressor, to avoid to relax a large flow of high pressure at the pressure of the column. It is also generalizable to all partial condensation devices.
• a flow containing carbon monoxide, hydrogen, methane and nitrogen 45 cools in exchanger 9 by heat exchange with a flow of carbon monoxide 1 and is sent to a methane scrubber column.
• the bottom liquid of the column C1 is sent to the top of the depletion column C2.
• the overhead gas of the C1 column enriched in hydrogen leaves the installation.
• the bottoms liquid from the exhaust column C2 is sent to a CO / C3 methane separation column.
• the bottom liquid of column C3 is returned to the top of column C1.
• the overhead gas from the column C3 is sent to an intermediate point of the denitrogenation column C4 where it separates into a carbon monoxide rich liquid in the tank and a nitrogen-rich gas at the top.
• the operation of the columns therefore corresponds essentially to that of the process of Figure 6 of Linde Reports on Science and Technology,
• a flow rate of impure carbon monoxide at a pressure of 2.6 bar is sent to the compressor V1, V2 to be compressed to a pressure between 25 and 45 bar, preferably between 35 and 40 bar to form the flow 5.
• This flow is divided into a part 7 which constitutes a production and another flow which is sent to the exchanger 9.
• a fraction 13 passes entirely through the exchanger before being divided in two.
• a first flow 55 is then divided into three flow rates 19, 21, 23.
• a first flow 19 serves to reboil the exhaust column C2, a second flow 23 serves to reboil the CO / methane C3 column, the two flows 19, 23 being thereby liquefied and the cooled flow rates 19, 23 are sent with the third flow 21 to an exchanger 17.
• the flow 23 is divided in two, a portion 25 being expanded in a valve 27 and then vaporized in the exchanger 17 and sent under gaseous form in the tank of the denitrogenation column C4.
• the remainder 26 of the flow 23 is expanded to a pressure of 2.6 bar and sent to a separator pot 35 after expansion in a valve.
• the flow rates 21, 19 are also expanded in valves and sent to the same separator pot 35. It will be readily understood that part of one of the flow rates 19, 21 could be vaporized and sent to the bottom of the denitrogenation column C4 in addition to or instead of the flow rate 25.
• the flow 57 of high pressure carbon monoxide is expanded in a valve 59 and then sent to the bottom of the denitrogenation column C4.
• the sending of high pressure carbon monoxide 57 expanded in the valve 59 is triggered if the flow rate of gaseous carbon monoxide 15,25 sent to the denitrogenation column is reduced by at least 5%, or even by at least 10% compared to the nominal flow.
• the gas 43 formed in the separator pot 35 is returned to the compressor
• the liquid of the separator pot 35 is divided into four.
• a part 1 is sent to a separator pot 33 where it forms a gaseous fraction 41 and a liquid fraction 31.
• the liquid fraction 31 vaporizes in the exchanger 17.
• the gaseous fraction 41 is heated in the exchanger 17 against the flow rates 19 , 21,
• Part 2 serves to sub-cool the methane wash column C1 before being mixed at the flow rate 41.
• Part 3 serves to condense the head of the column CO / methane C3 where it vaporizes and is then returned to the compressor V1.
• the fourth portion 37 is mixed with the bottom liquid 29 of the denitrogenation column and serves to cool the head thereof.
• the formed flow 39 is returned to the compressor V1.
• a flow 11 cools partially in the exchanger 9, is expanded in a turbine T, cools in the exchanger 17 as flow 15 and is sent to the bottom of the denitrogenation column C4.

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• Engineering & Computer Science (AREA)
• Physics & Mathematics (AREA)
• Mechanical Engineering (AREA)
• Thermal Sciences (AREA)
• General Engineering & Computer Science (AREA)
• Separation By Low-Temperature Treatments (AREA)
• Carbon And Carbon Compounds (AREA)

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• 2006
  • 2006-12-21 FR FR0655770A patent/FR2910602B1/fr not_active Expired - Fee Related
• 2007
  • 2007-12-12 WO PCT/FR2007/052486 patent/WO2008078040A2/fr active Application Filing
  • 2007-12-12 US US12/519,990 patent/US8555673B2/en active Active
  • 2007-12-12 EP EP07871916.8A patent/EP2140216B1/de active Active
  • 2007-12-12 CN CN2007800477659A patent/CN101568788B/zh active Active

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