EP0539268A1 - Verfahren zur Entfernung von Wasserstoff bei der kryogenen Destillation zwecks Erzeugung von hochreinem Stickstoff - Google Patents

Verfahren zur Entfernung von Wasserstoff bei der kryogenen Destillation zwecks Erzeugung von hochreinem Stickstoff Download PDF

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EP0539268A1
EP0539268A1 EP92402799A EP92402799A EP0539268A1 EP 0539268 A1 EP0539268 A1 EP 0539268A1 EP 92402799 A EP92402799 A EP 92402799A EP 92402799 A EP92402799 A EP 92402799A EP 0539268 A1 EP0539268 A1 EP 0539268A1
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Prior art keywords
distillation column
liquid
nitrogen
column
fraction
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French (fr)
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EP0539268B1 (de
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Bao Ha
Wilfrid Petrie
François Venet
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Liquid Air Engineering Corp Canada
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Liquid Air Engineering Corp Canada
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J3/04—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 for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04296—Claude expansion, i.e. expanded into the main or high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
    • F25J3/0219—Refinery gas, cracking gas, coke oven gas, gaseous mixtures containing aliphatic unsaturated CnHm or gaseous mixtures of undefined nature
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    • 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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    • 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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    • 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
    • F25J3/04—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 for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J3/04—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 for air
    • F25J3/04406—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 for air using a dual pressure main column system
    • F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
    • F25J2200/06—Processes or apparatus using separation by rectification in a dual pressure main column system in a classical double column flow-sheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/20—Processes or apparatus using separation by rectification in an elevated pressure multiple column system wherein the lowest pressure column is at a pressure well above the minimum pressure needed to overcome pressure drop to reject the products to atmosphere
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/52—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the high pressure column of a double pressure main column system
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/42—Separating low boiling, i.e. more volatile components from nitrogen, e.g. He, H2, Ne
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/42—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen

Definitions

  • the present invention relates to a process for removing hydrogen by cryogenic distillation in the production of high purity nitrogen.
  • contaminate hydrogen in nitrogen is removed by passing compressed atmospheric feed air through a catalytic bed at a temperature of about 250 to 500°F, whereby the hydrogen reacts with oxygen to form water and carbon dioxide which are then removed in a subsequent step either by adsorption or by reversing exchangers. Removal of hydrogen by this method is undesirable, however, due to the expense of the catalyst and the possible poisoning of the catalyst by other impurities present in air, such as, for example, sulfur-containing compounds. Furthermore, the catalytic reactor and the equipment associated therewith are very expensive and represent a significant portion of the total required expense.
  • Figure 1 represents a flow sheet for hydrogen removal by cryogenic distillation in the production of high purity nitrogen, where liquid product is extracted at the bottom of the second column as well as the gaseous product.
  • Figure 2 represents a flow sheet for hydrogen removal by cryogenic distillation in the production of high purity nitrogen, where nitrogen recovery is enhanced with a nitrogen cycle.
  • Oxygen-rich liquid in the bottom of the first column is vaporized by indirect heat exchange with a compressed nitrogen cycle which is condensed and expanded at the top of the first column to increase its reflux and reboil.
  • Figure 3 represents a flow sheet for hydrogen removal by cryogenic distillation in the production of high purity nitrogen, where the refrigeration requirement is achieved by expanding a fraction of compressed air in a turbine before being fed to the first distillation column.
  • the nitrogen recovery is enhanced by condensing an air stream in the bottom reboiler of the first distillation column.
  • a method for removing hydrogen by cryogenic distillation in the production of high purity nitrogen without using a catalytic reactor containing a catalyst.
  • the present invention provides a double column process wherein a first distillation column is used to extract a first fraction of nitrogen product in liquid form. A very small amount of hydrogen is present in this liquid due to the high relative volatility of hydrogen as compared to nitrogen. Then, this liquid nitrogen is fed to a second distillation column, where it is further purified to yield a high purity nitrogen product at the bottom of the distillation column.
  • the present invention provides a process for removing hydrogen by cryogenic distillation in the production of high purity nitrogen, which entails several steps.
  • compressed air or a feed mixture comprising oxygen and nitrogen which is substantially free of water and carbon dioxide and which has been cooled to about the dew point thereof is fed to the bottom of a first distillation column which is operated at a pressure such that heavy air components are separated from nitrogen.
  • nitrogen is produced at the top of the distillation column as a liquid, and a liquid stream rich in oxygen is produced at the bottom of the distillation column.
  • the first distillation column be operated at a pressure of about 4 to 12 bar in order to effectively separate the heavy air components, such as oxygen and argon, from nitrogen.
  • This air normally contains up to about 20 vpm of hydrogen.
  • the first distillation column produces at the top a liquid product rich in nitrogen.
  • the term “heavy air components” refers to all components of air which have a lower volatility than nitrogen, i.e. its vapor pressure is lower than the vapor pressure of nitrogen at the same temperature.
  • the term “light air components” as used in the present specification is intended to include all components of air which have a higher volatility than nitrogen, i.e. its vapor pressure is greater than the vapor pressure of nitrogen at the same temperature.
  • oxygen and argon are examples of heavy air components
  • hydrogen and helium are examples of light air components.
  • the liquid nitrogen is expanded at the top of the first distillation column into a second distillation column at an intermediate level, and the second distillation column is operated at a pressure sufficiently lower than the pressure of the first distillation column to provide a sufficient temperature difference in the condenser-reboiler located between the two columns.
  • the liquid stream rich in oxygen is vaporized in the overhead condenser of the second distillation column to form a condensate of a major fraction of the gas at the top of the second distillation column, and then the condensate is returned to the top of the second column as reflux.
  • the second distillation column may be operated at any pressure lower than the pressure of the first distillation column to provide a sufficient temperature difference in the condenser-reboiler separating the two columns. It is preferred, however, that the second distillation column be at a pressure at least about 0.4 bars lower than the pressure of the first distillation column. It is even more preferred, however, if the second distillation column is at a pressure about 0.6 bar lower than the pressure of the first distillation column.
  • the phrase containing "substantially all light air components” means that at least 99.99% of all light air components are contained therein. Also, as used in the present specification, the phrase containing “substantially no light air components” means that no more than 0.01% of all light air components are contained therein.
  • liquid product may also be extracted at the bottom of the second distillation column as well as the gaseous product. This is represented in Figures 2 and 3.
  • a subcooler can be added to subcool the bottom liquid of the first distillation column against the outgoing gaseous product and the residual stream rich in oxygen. This is represented in Figure 2.
  • the refrigeration requirement can be achieved by expanding the stream rich in oxygen, or expanding the gaseous nitrogen product or by adding liquid to the process in a liquid assist or by expanding a fraction of the feed air.
  • the present invention may be used in conjunction with other processes whenever the removal of a light product from a mixture containing heavier components is required.
  • the present invention may also be used advantageously in conjunction with any process where light products are to be removed from mixtures of heavier components.
  • the present process may be used to remove carbon monoxide from mixtures also containing heavier hydrocarbons, such as methane (CH4).
  • CH4 methane
  • the process is applicable to several hydrocarbon mixtures containing lighter impurities.
  • the present invention may be used with any of these to effect removal of the light component.
  • reaction mixtures which contain a lighter component and one or more heavy components.
  • the light component in the reaction mixture may be an unreacted raw material.
  • the lighter component in the reaction mixture may be one of the reaction products.
  • the present process may be used to advantage with any of these processes to remove light components.
  • the present process in conjunction with processes producing a light product from a mixture containing mainly the light product, one or more heavier components and with traces of a lighter impurity. It is more preferred if the lighter impurity is present in the mixture only in an amount of up to about 1% by volume, most preferably only up to about 0.5% by volume.
  • a process for producing or removing a light or more volatile product from a mixture mainly containing the light or more volatile product and heavier or less volatile components and traces of lighter impurities which are lighter or have a higher volatility than the light product.
  • the present invention provides a process for removing a light product from a mixture mainly comprising a light product, one or more heavier components and a trace of one or more lighter impurities by cryogenic distillation, which comprises:
  • the lighter impurities are accumulated at the top of the first column. Some of the lighter impurities are soluble in the light-product liquid, and some of the lighter impurities remain in a vapor fraction called the non-condensible stream. This stream is removed from the column along with the lighter impurities contained therein.
  • the term "the greater portion of” refers to any portion greater than about 50% by volume. However, it is preferred that the greater portion be in excess of about 80%, even more preferably in excess of about 99% by volume.
  • the present invention provides an efficient means for separating a light product, one or more heavier components and one or more lighter impurities.
  • the feed mixture mainly contains the light product and one or more heavier components.
  • the feed mixture contains from 50 to 99.99% by volume of light product and one or more heavier components. It is preferred, however, if the feed mixture contains from 75 to 99.99% by volume of light product and one or more heavier components.
  • the one or more lighter impurities are present in an amount of up to about 1% by volume, preferably not more than about 0.5% by volume.
  • the term “light product” means the mixture component having the higher volatility.
  • the term “heavier components” means the mixture component or components having the lowest volatility.
  • the term “lighter impurities” means the impurity component or components having an intermediate volatility and which are present in amounts of only up to about 1% by volume.
  • the "trace" of lighter impurities is intended to mean a minor amount of generally less than 1% by volume.
  • non-condensible is intended to mean non-condensible under conditions prevailing outlet for the top condenser of both columns.
  • a cooled, compressed, cleaned and dried feed stream containing light product, one or more heavier components and a trace of one or more lighter impurities, such as atmospheric air, is fed via conduit (10) to heat exchange means (11), and then to the high pressure column (13) via conduit (12).
  • a nitrogen-rich liquid is fed from the high pressure column (13) to the low pressure column (14) via conduit (16) for feed.
  • liquid nitrogen (LIN) may be removed from the column as liquid product from the bottom of the low pressure column (14).
  • Non-condensible material is withdrawn from the column at condenser-reboiler (15), and from the overhead condenser (80) of the low pressure column.
  • Waste gas is removed from the overhead condenser (80) via conduits (21) and (22), optionally through subcooler (18), to heat exchange means (11), where it exits the process via conduit (28).
  • This waste originates from a bottom stream (17) withdrawn from the high pressure column, wherein after it is optionally passed through subcooler (18) and to the overhead condenser (80) via conduit (20).
  • a cooled, compressed, cleaned and dried feed stream containing light product, one or more heavier components and a trace of one or more lighter impurities, such as atmospheric air, and which is close to the dew point is fed to an intermediate location of a high pressure column (13), wherein an oxygen-rich stream separates at the bottom and a nitrogen-rich stream at the top.
  • a liquid nitrogen stream is extracted at the top of the high pressure column (13) and fed to the low pressure column (14) via conduit (16) at an intermediate location.
  • a minor gaseous fraction or non-condensible containing some lighter impurities is removed at the top of the high pressure columns (13) via conduit (30).
  • lighter impurities are removed via the non-condensible stream at the top of the low pressure column (14) with the bottom fraction being substantially free, i.e., less than about 0.5% by volume thereof, of lighter impurities.
  • Nitrogen product can be extracted from the bottom of the low pressure column as a liquid (LIN) via conduit (24). Gaseous nitrogen product is extracted from the column via conduit (19) and rewarmed in exchanger (11). A portion of this product is recovered via conduit (54) and the remaining portion is compressed in compressor (60). A fraction of this compressed stream may be recovered as product via conduit (57). The remaining fraction is sent to the high pressure column reboiler (52) via conduit (51) where it condenses to provide the reboil for the high pressure column.
  • LIN liquid
  • Nitrogen product can be extracted from the bottom of the low pressure column as a liquid (LIN) via conduit (24). Gaseous nitrogen product is extracted from the column via conduit (19) and rewarmed in exchanger (11). A portion of this product is recovered via conduit (54) and the remaining portion is compressed in compressor (60). A fraction of this compressed stream may be recovered as product via conduit (57). The remaining fraction is sent to the high pressure column reboiler (52) via conduit (51) where it condenses to provide the
  • the condensed recycle stream is fed via conduit (53) from the reboiler to the top of the high pressure column to provide extra reflux for the high pressure column.
  • An oxygen-rich stream is passed from the bottom of the high pressure column (13) via conduit (17) to the overhead condenser (80) of the low pressure column, whereby it vaporizes and passes to the exchanger (11), and is rewarmed.
  • the rewarmed stream is then fed to an expander and then to an exchanger where it is used to provide required refrigeration and then exits as waste.
  • fraction of a cooled, compressed, cleaned and dried feed stream is fed via conduit (73) to the bottom reboiler (52) of the distillation column (13) where it is liquified, the liquified feed stream is then fed to the high pressure column (13).
  • Another fraction of the cooled, compressed, cleaned and dried feed stream is expanded via expander (71) into the high pressure column (13), wherein in the top section thereof pure nitrogen and lighter impurities are extracted and in the bottom section oxygen-rich liquid is extracted. Some lighter impurities may be removed via conduit (30).
  • Liquid nitrogen fraction is extracted at the top of the high pressure column and fed via conduit (16) to an intermediate stage of the low pressure column.
  • the gaseous nitrogen fraction which forms at the top of the high pressure column is condensed in reboiler (15) to provide reboil for the low pressure column.
  • the low pressure column (14) further purifies liquid nitrogen feed and a liquid product may be recovered at the bottom of the low pressure column via conduit (24), which is free of lighter impurities.
  • Conduit (19) affords recovery of gaseous nitrogen which is free of lighter impurities.
  • the remaining lighter impurities are removed via conduit (31) and exit at the top of the low pressure column.
  • Oxygen-rich liquid from the bottom of the high pressure column is transferred via conduit (17) to the top condenser (80) of the low pressure column, where it is vaporized and leaves the process via conduit (21), (22) and (28), optionally passing through subcooler (10), and then passing through exchanger (11)
EP92402799A 1991-10-15 1992-10-14 Verfahren zur Entfernung von Wasserstoff bei der kryogenen Destillation zwecks Erzeugung von hochreinem Stickstoff Expired - Lifetime EP0539268B1 (de)

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US77550391A 1991-10-15 1991-10-15
US775503 1991-10-15

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EP0539268B1 EP0539268B1 (de) 1997-11-19

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EP (1) EP0539268B1 (de)
JP (1) JP2983393B2 (de)
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0924486A2 (de) * 1997-12-19 1999-06-23 The BOC Group plc Lufttrennung
EP1080763A1 (de) * 1999-09-03 2001-03-07 Air Products And Chemicals, Inc. Verfahren zur Reiningung einer Hauptkomponente in einer Mischung dieser Komponete mit leichter und schwerer flüchtigen Komponenten
EP1080765A1 (de) * 1999-09-03 2001-03-07 Air Products And Chemicals, Inc. Mehrstufige Rektifikation
EP1300640A1 (de) * 2001-10-04 2003-04-09 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung von hoch reinem Stickstoff durch Tieftemperaturzerlegung von Luft
CN102506559A (zh) * 2011-09-28 2012-06-20 开封东京空分集团有限公司 多段精馏制取高纯氮气空分工艺
CN102589250A (zh) * 2012-02-14 2012-07-18 开封黄河空分集团有限公司 一种由空气分离制取氮气的工艺
CN107062800A (zh) * 2017-04-21 2017-08-18 上海启元特种气体发展有限公司 一种超纯氮除氢的方法及其装置
CN107560318A (zh) * 2017-09-22 2018-01-09 杭州杭氧股份有限公司 一种低温精馏法氮气提纯装置及提纯方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7360909B2 (ja) * 2019-11-18 2023-10-13 東洋エンジニアリング株式会社 水素分離方法および水素分離装置

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US4902321A (en) * 1989-03-16 1990-02-20 Union Carbide Corporation Cryogenic rectification process for producing ultra high purity nitrogen
EP0485612A1 (de) * 1990-05-31 1992-05-20 Kabushiki Kaisha Kobe Seiko Sho Verfahren und vorrichtung zur herstellung hochreinen stickstoffes
US5123947A (en) * 1991-01-03 1992-06-23 Air Products And Chemicals, Inc. Cryogenic process for the separation of air to produce ultra high purity nitrogen

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JPH0814335B2 (ja) * 1989-08-10 1996-02-14 マスコ コーポレーション 押下げ変換装置を有する２つの出口をもつ水栓

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US4902321A (en) * 1989-03-16 1990-02-20 Union Carbide Corporation Cryogenic rectification process for producing ultra high purity nitrogen
EP0485612A1 (de) * 1990-05-31 1992-05-20 Kabushiki Kaisha Kobe Seiko Sho Verfahren und vorrichtung zur herstellung hochreinen stickstoffes
US5123947A (en) * 1991-01-03 1992-06-23 Air Products And Chemicals, Inc. Cryogenic process for the separation of air to produce ultra high purity nitrogen

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0924486A2 (de) * 1997-12-19 1999-06-23 The BOC Group plc Lufttrennung
EP0924486A3 (de) * 1997-12-19 1999-09-29 The BOC Group plc Lufttrennung
US6141989A (en) * 1997-12-19 2000-11-07 The Boc Group Plc Air separation
EP1080763A1 (de) * 1999-09-03 2001-03-07 Air Products And Chemicals, Inc. Verfahren zur Reiningung einer Hauptkomponente in einer Mischung dieser Komponete mit leichter und schwerer flüchtigen Komponenten
EP1080765A1 (de) * 1999-09-03 2001-03-07 Air Products And Chemicals, Inc. Mehrstufige Rektifikation
EP1300640A1 (de) * 2001-10-04 2003-04-09 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung von hoch reinem Stickstoff durch Tieftemperaturzerlegung von Luft
US6708523B2 (en) 2001-10-04 2004-03-23 Linde Aktiengesellschaft Process and apparatus for producing high-purity nitrogen by low-temperature fractionation of air
CN100334412C (zh) * 2001-10-04 2007-08-29 林德股份公司 通过低温空气分馏来生产高纯度氮的工艺和设备
CN102506559A (zh) * 2011-09-28 2012-06-20 开封东京空分集团有限公司 多段精馏制取高纯氮气空分工艺
CN102589250A (zh) * 2012-02-14 2012-07-18 开封黄河空分集团有限公司 一种由空气分离制取氮气的工艺
CN107062800A (zh) * 2017-04-21 2017-08-18 上海启元特种气体发展有限公司 一种超纯氮除氢的方法及其装置
CN107560318A (zh) * 2017-09-22 2018-01-09 杭州杭氧股份有限公司 一种低温精馏法氮气提纯装置及提纯方法

Also Published As

Publication number Publication date
JP2983393B2 (ja) 1999-11-29
EP0539268B1 (de) 1997-11-19
DE69223217D1 (de) 1998-01-02
JPH05302783A (ja) 1993-11-16
DE69223217T2 (de) 1998-05-28

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