EP4244559A2 - Procédé cryogène pour la récupération de matière valorisable à partir d'un gaz d'alimentation riche en matière valorisable - Google Patents

Procédé cryogène pour la récupération de matière valorisable à partir d'un gaz d'alimentation riche en matière valorisable

Info

Publication number
EP4244559A2
EP4244559A2 EP21823483.9A EP21823483A EP4244559A2 EP 4244559 A2 EP4244559 A2 EP 4244559A2 EP 21823483 A EP21823483 A EP 21823483A EP 4244559 A2 EP4244559 A2 EP 4244559A2
Authority
EP
European Patent Office
Prior art keywords
hydrogen
product
rich
column
nitrogen
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP21823483.9A
Other languages
German (de)
English (en)
Inventor
Norbert Peters
Hans Schmidt
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xenon Holding GmbH
Original Assignee
Xenon Holding GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xenon Holding GmbH filed Critical Xenon Holding GmbH
Publication of EP4244559A2 publication Critical patent/EP4244559A2/fr
Pending legal-status Critical Current

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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
    • F25J3/0209—Natural gas or substitute natural gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—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
    • 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
    • F25J3/0228—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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    • 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
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    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
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    • 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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    • 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
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    • 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
    • F25J3/028—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 noble gases
    • F25J3/029—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 noble gases of helium
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    • 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
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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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/40—Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
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    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
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    • F25J2210/60—Natural gas or synthetic natural gas [SNG]
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    • F25J2215/14—Carbon monoxide
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    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
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    • 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
    • F25J2270/902—Details about the refrigeration cycle used, e.g. composition of refrigerant, arrangement of compressors or cascade, make up sources, use of reflux exchangers etc.

Definitions

  • the invention relates to a cryogenic process for recovering valuable substances, in particular hydrogen, from a hydrogen-rich feed gas, preferably hydrogen-rich natural gas, with hydrocarbons having two or more carbon atoms, methane and nitrogen being separated off in at least 3 separation columns.
  • a hydrogen-rich feed gas preferably hydrogen-rich natural gas
  • Hydrogen is usually obtained from residual gas streams from chemical processes, such as reforming or cracking processes.
  • the hydrogen from these residual gas streams is enriched and/or isolated by membrane adsorbers and/or pressure swing adsorbers.
  • These residual gas streams generally include methane, hydrocarbon mixtures of various chain lengths, preferably light hydrocarbons, carbon monoxide and carbon dioxide.
  • the aim of the present invention is therefore to provide a comprehensive process that has the capacity of large-scale plants, efficiently and inexpensively separates large quantities of a hydrogen-rich feed gas, in particular a hydrogen-rich natural gas, into the valuable materials contained therein and, if necessary, after adjusting the purity for provides additional processes.
  • a hydrogen-rich feed gas in particular a hydrogen-rich natural gas
  • a holistic process is advantageous here, which separates all the valuable substances present in the feed gas as efficiently, cost-effectively and comprehensively as possible from one another on an industrial scale and further uses or processes or as an energy source.
  • such a process is also advantageous for hydrogen-rich feed gases that occur industrially on a large scale, in particular against the background of the increasing use of hydrogen as an energy source in the automotive and other industrial sectors.
  • a cryogenic process for recovering valuable substances, in particular hydrogen, from a hydrogen-rich feed gas, preferably a hydrogen-rich natural gas, is described, with hydrocarbons having two or more carbon atoms being separated off in a first separation column and methane being separated off in a second separation column is, and nitrogen is separated in a third separation column.
  • the invention relates to a cryogenic process for recovering valuable substances, in particular hydrogen, from a hydrogen-rich feed gas, preferably a hydrogen-rich natural gas, comprising the following steps: a) in a first separation column (T1), in particular a rectification column, hydrocarbons m separated with two or more carbon atoms, b) methane is separated off in a second separation column (T2), in particular a rectification column, and c) in a third separating column (T3), in particular a rectification column, nitrogen is separated off, with the hydrogen-rich feed gas being fed to the separating columns T1 to T3 according to steps a) to c) after optional pre-cleaning and in the separating columns into a liquid fraction, the Bottom product, and a gas fraction, the top product, is separated.
  • T1 first separation column
  • T2 second separation column
  • T3 in particular a rectification column
  • feed gas means a hydrogen-rich raw gas with a hydrogen content of 50% by volume or higher, which comes from an industrial process or from a natural natural gas source, which includes the valuable components hydrogen, methane, carbon with two or more carbon atoms and nitrogen and which serves as the starting gas of the cryogenic process according to the invention.
  • the term input fraction means the gas arriving at the respective separation column, which gas is passed through the corresponding separation column and is thereby separated into at least 2 fractions, a top fraction and a bottom fraction.
  • Natural gas in the sense of this invention means a gas that is produced by naturally occurring processes and that has arisen below the surface of the earth or in the interior of the earth.
  • the hydrogen-rich natural gas preferably comes from a natural gas source.
  • the hydrogen-rich feed gas preferably hydrogen-rich natural gas, has a hydrogen content of 50 to 99.9% by volume, preferably 70 to 99.9% by volume hydrogen, particularly preferably 90 to 99.9% by volume hydrogen.
  • nitrogen, methane and noble gases in particular helium, neon and argon, and hydrocarbons with two or more carbon atoms can be included in the feed gas, in particular natural gas, as further components.
  • Carbon dioxide can also be included in lower concentrations, in particular between 0 and 10% by volume, while carbon monoxide and sulfur components can be present in concentrations between 0 and 0.5% by volume.
  • the hydrogen-rich feed gas in particular the hydrogen-rich natural gas, has as its main components a hydrogen content of between 50 and 99.9% by volume, a methane content of between 0.02 and 40% by volume and a nitrogen content of between 0 02 and 30% by volume, preferably a hydrogen content of at least 70% by volume, a methane content of at most 20% by volume and a nitrogen content of at most 20% by volume, particularly preferably a hydrogen content of at least 90% by volume %, a methane content of no more than 10% by volume and a nitrogen content of no more than 10% by volume,
  • the first, second, third, fourth and fifth separation column is advantageously a rectification column.
  • the cooling is preferably provided at least partially by one or more cooling circuits.
  • the hydrogen-rich feed gas preferably the hydrogen-rich natural gas
  • the separation columns preferably the rectification columns
  • the refrigerant or refrigerant mixture in at least one heat exchanger (E1).
  • the raw gas (BO), i.e. the hydrogen-rich feed gas, in particular the hydrogen-rich natural gas from the natural gas well, is pre-cleaned (R) by removing one or more components of the feed gas that would freeze out in the low-temperature part of the plant.
  • Such components are in particular selected from the group consisting of water, carbon dioxide, hydrogen sulfide, mercaptans and mercury compounds, in particular mercury, or combinations thereof. These components can be removed by means of adsorption and/or absorption processes as part of the pre-cleaning.
  • natural natural gas sources in particular hydrogen-rich natural gas sources, contain water that has to be removed as part of a pre-cleaning, pre-treatment or drying process.
  • natural gas sources that are already very low in carbon dioxide, hydrogen sulfide, mercaptans and/or mercury compounds, in particular mercury, or possibly none of these components at all - at least in partial fractions of the production - further pre-cleaning can be dispensed with if necessary will.
  • Hydrogen-rich feed gases from industrial processes that contain the same components are treated accordingly.
  • a hydrogen-rich raw gas from a natural gas source is pre-cleaned and thereby at least the water component is removed, preferably carbon dioxide, hydrogen sulfide, mercaptans and/or mercury compounds, in particular mercury, are removed by pre-cleaning.
  • feed gas that does not contain any of the components described above that are to be removed in the course of the pre-cleaning, pre-cleaning, pre-treatment and/or drying can be dispensed with.
  • the raw gas in particular the hydrogen-rich natural gas
  • the valuable substances contained in the raw gas in particular hydrogen, hydrocarbons with two or more carbon atoms, methane, nitrogen, are separated from the raw gas or pre-cleaned raw gas in the separating columns T1 to T3, preferably in rectification columns. It is advantageous to compress the raw gas to a pressure of between 20 and 50 bar before it is liquefied. In particular, in the case of the comparatively valuable component hydrogen, extraction at high pressure is desirable, since the hydrogen can usually be used further, e.g. B. compression, is supplied.
  • the liquid phase is referred to as the bottom product and the gas phase as the top product.
  • the bottom product from the first removal column T1 preferably the first rectification column, in particular C2, C3 hydrocarbons and higher hydrocarbons, in a further fractionation, i.e. a fourth removal column T4, preferably a fourth rectification column, to ethane gas (B3) and LPG (B2) fractionated.
  • the bottom product of the separating column T1 can initially serve as a cold supplier in E1 and possibly, after throttling, be fed into the separating column T4 in two phases.
  • a partial stream of the hydrogen-rich feed gas, after optional pre-cleaning R(B1), can be fed directly into the lower part of the separation column T1, bypassing the heat exchanger E1.
  • the reboiler of the separating column T1 is at least partially relieved.
  • the fraction containing at least methane, nitrogen and hydrogen (top product) is taken off.
  • This is cooled further in the heat exchanger E1 and then fed to the second separating column T2, preferably the second rectification column, via a line in which an expansion valve can optionally be provided.
  • a substream of the top stream of the removal column T1 can be fed directly into the lower part of the removal column T2, bypassing the heat exchanger E1.
  • the result of this is that the reboiler of the separating column T2 is at least partially relieved (not shown in FIG. 1).
  • the top condenser is cooled by the heat exchanger E1 of the first separation column T1, preferably the rectification column, according to the invention using a refrigerant or refrigerant mixture or a partial flow of the refrigerant or refrigerant mixture.
  • the top condensers of all separation columns can be designed either as plate exchangers, preferably as multi-stream plate exchangers, as coiled heat exchangers, preferably as multi-stream coiled exchangers, TEMA exchangers, series of coiled exchangers and/or plate exchangers connected in series and in or above the respective separation column T, preferably rectification column T, can be arranged, with an arrangement above the rectification column making a return pump obsolete.
  • the contamination of the respective top products can be kept within narrow limits.
  • the ethane content of the fraction taken off overhead in the separation column T1 can be adjusted almost as desired, namely between approx. 10 ppmV to a few vol%, preferably less than 2% vol, particularly preferably less than 1% vol.
  • the methane content in the bottom product of the separating column T1 can be set almost at will, namely between about 1 ppm to a few% by volume, preferably less than 2% by volume, particularly preferably less than 1% by volume.
  • the valuable materials separated at the top of the first separation column T1, preferably rectification column, comprising at least one or more valuable materials from the group consisting of methane, nitrogen and hydrogen, are, after further cooling in the heat exchanger E1, via a line in which an expansion valve can optionally be provided, fed to the separating column T2, preferably rectification column, and separated therein into a liquid fraction and a gas fraction.
  • a substream of the top stream of the removal column T2 can be fed directly into the lower part of the removal column T3, bypassing the heat exchanger E1.
  • the result of this is that the reboiler of the separating column T3 is at least partially relieved (not shown in FIG. 1).
  • the top condenser E1 of the second separation column T2 preferably the rectification column, is cooled by a refrigerant or refrigerant mixture or a partial stream of the refrigerant or refrigerant mixture.
  • the methane-rich bottom product from the second separation column T2, preferably rectification column is either warmed up in the heat exchanger (E1) and compressed as methane gas (B4) or further cooled in the heat exchanger (E1), expanded and recovered as LNG.
  • the valuable materials separated at the top of the separation column T2, preferably rectification column, comprising at least one or more valuable materials from the group consisting of nitrogen, helium and hydrogen, after further cooling, are transferred to the third separation column T3 via a line in which an expansion valve can optionally be provided, preferably rectification column, and separated in this into a liquid and a gas fraction.
  • a portion of the nitrogen-rich bottom product of the separation column T3 can be expanded, heated in the heat exchanger (E1) and fed into the refrigeration circuit of E1 as a refrigerant or a component of the refrigerant.
  • the nitrogen-rich bottom product can also be heated in E1 without expansion and used further as high-pressure nitrogen (B5).
  • the bottom stream from the separation column T3 (high-pressure LlN) can be expanded and used as the first refrigerant stage for the liquefaction of the hydrogen or helium.
  • carbon monoxide is contained in the raw gas, this is enriched in the nitrogen-rich bottom product of the third separation column T3, preferably rectification column, and can preferably be converted to carbon dioxide at the warm end of the process by metering in oxygen in an additional process unit. Nitrogen with small amounts of carbon dioxide is obtained as a reusable material, which can be used and/or supplied to other processes.
  • a fifth removal column in particular a hydrogen removal column (T5), preferably rectification column
  • the hydrogen-rich top product from the third separation column T3, preferably the rectification column is heated (B6) in the heat exchanger (E1), compressed and fed into a pipeline.
  • it can be cleaned of residual impurities in a standard hydrogen liquefaction plant, liquefied and stored, preferably in special vacuum-insulated tanks.
  • the top product can post-hydrogen from the removal column T3, preferably the rectification column, in a special unit the state of the art, are first cleaned by adsorptive means, then liquefied and stored, preferably in vacuum-insulated special tanks.
  • the respective products are adjusted in their purity as valuable materials.
  • the methane-rich bottom product of the separation column T2 the hydrogen-rich top product, the nitrogen-rich bottom product of the separation column T3 and the ethane-rich top product of the separation column T4 are converted into LPG product (B2) or ethane product (B3) or methane product in accordance with the cold supply in E1 (B4) or nitrogen product (B5) or
  • Hydrogen product (B6) as recyclable materials in their purity and then to make them available to other processes or recycling/uses.
  • the products of the separation column T5 i.e. the hydrogen bottom product or helium overhead product, are likewise adjusted in their purity in separation column T5.
  • the top product helium is first cleaned by adsorptive means, then liquefied and stored, preferably in vacuum-insulated special tanks.
  • the bottom product hydrogen is adsorptively cleaned and stored, preferably in vacuum-insulated special tanks.
  • the condensers of the separating columns, preferably rectification columns, T1 to T4 and the reboilers of T1 to T3 are connected to E1 or integrated into E1.
  • the at least one heat exchanger unit E1 used in the method according to the invention is designed as a multi-flow plate exchanger or coiled exchanger, in particular as a series of coiled exchangers and/or plate exchangers connected in series, preferably in multiple subdivisions according to the temperature profile of the separation process, in order to achieve exergetically favorable temperature differences over the entire cooling ensure and preferably in multiple parallel circuits - depending on the capacity of the system.
  • the cold supply of the separation process of the separation columns, preferably rectification columns, (T1 to T4) according to the method according to the invention is either a) via a nitrogen expander circuit with at least one expander-compressor (Xi-Ci), the compressors Ci serving as the final stages of the circuit compression .
  • Nitrogen as a refrigerant component can preferably be provided from the nitrogen product (B5), alternatively from the bottom product of T3, or b) via an expander refrigeration cycle m ith nitrogen and methane as components analogous to a), the expander compressor X2 -C2 can also be replaced by a Joules-Thompson expansion valve.
  • Methane can also be used as Refrigerant components are preferably made available from the methane product (B4), alternatively from the bottom product of T2, or c) via a mixture circuit which consists of at least two components selected from the group consisting of nitrogen, methane, ethane, propane, i-butane, n-butane, i-pentane, n-pentane, hexane and heptane, which are preferably selected according to the process optimization for minimum exergy losses in E1, or d) via a series connection of selected refrigeration circuits a) to c) according to the process optimization for minimum Exergy losses in E1 .
  • a mixture circuit which consists of at least two components selected from the group consisting of nitrogen, methane, ethane, propane, i-butane, n-butane, i-pentane, n-pentane, hexane and heptane, which are
  • cryogenic method according to the invention for recovering valuable substances from hydrogen, hydrocarbons with two or more hydrocarbons, methane and nitrogen from hydrogen-rich feed gas, in particular hydrogen-rich natural gas, and further advantageous configurations of the same are explained in more detail below with reference to the exemplary embodiment illustrated in the figure.
  • FIG. 1 schematically shows the cryogenic process according to the invention. Optional further processing steps are shown in dashed lines.
  • the following reference marks and abbreviations are used:
  • This cryogenic process is carried out with rectification columns.
  • the starting fraction containing at least methane, nitrogen and hydrogen is fed via line 1 to a pre-purification unit R which may be provided.
  • a pre-purification unit R which may be provided.
  • this is optionally precompressed to a pressure of between 20 and 50 bar.
  • water, carbon dioxide and mercury compounds, in particular mercury are present, carbon dioxide and mercury removal and drying are generally carried out. If sulfur components are present, these are also removed in the course of the pre-cleaning.
  • the starting fraction of this type--if appropriate pretreated-- is then fed via line 2 to the heat exchanger E1, where it is cooled and partially condensed.
  • the heat exchanger E1 is usually designed as a plate heat exchanger or as a coiled heat exchanger. In the case of correspondingly large capacities, a plurality of heat exchangers arranged parallel to one another and/or one behind the other are optionally provided.
  • the cooling and liquefaction of the input fraction takes place against at least one refrigeration circuit of any design, which is only shown schematically in the figure by the line sections 21 to 27, which will be discussed in more detail below.
  • This refrigeration circuit is preferably designed as an expander or mixture circuit.
  • the cooled and possibly partially condensed starting fraction is fed to the rectification column T1 (ethane separation column) via line 3, in which an expansion valve a can be provided, and is separated there into a liquid fraction and a gas fraction.
  • the hydrogen-rich feed gas in particular the hydrogen-rich natural gas, (B1) contains heavy hydrocarbons
  • these can be fed to the heat exchanger E1 with the ethane-rich bottom product from the rectification column T1 via line 6, heated and then via line 16, in which an expansion valve e can be provided , the to the rectification column T4 (propane separation column) and separated into an ethane product as a top product of the rectification column T4 (B3) and an LPG (B2) as a bottom product of the rectification column T4.
  • line 6 can merge directly into line 16, bypassing heat exchanger E1.
  • Part of the input fraction can also be fed directly as stripping gas into the rectification column T1, bypassing the heat exchanger E1, in order to at least partially relieve the pressure on the reboiler.
  • a methane-rich liquid fraction with a nitrogen content of typically less than 3% by volume is drawn off from the bottom of the rectification column T2 via line 7 and heated in the heat exchanger E1 and fed to its further use as the methane product (B4).
  • the methane-rich liquid fraction can be supercooled against the refrigerant or refrigerant mixture of the refrigerant circuit in E1 and fed to a storage tank S via line 8 as an LNG product after expansion in valve f.
  • Tank return gas occurring within the storage tank S can be withdrawn from the storage tank S, if necessary compressed in one or more stages and discharged at the plant boundary.
  • the tank return gas can also be fed to a fuel gas system.
  • the nitrogen-rich bottom product of T3 can either be heated in E1 via line 12, which then merges into line 14, and be used further as nitrogen product (B5), or at least a partial stream can be expanded to the pressure of the refrigeration circuit in throttle valve h and used there as refrigeration or at least as part of the refrigerant.
  • the nitrogen-rich bottom product of T3 can also be fed via line 12 to the hydrogen liquefaction plant and the helium liquefaction plant, expanded and used there as a refrigerant.
  • the hydrogen-rich top product from T3 is fed via line 11 to heat exchanger E1, where it is heated and is available for further use as hydrogen product (B6).
  • the hydrogen product can either be compressed and fed to a pipeline or, possibly after compression, fed to a standard hydrogen liquefaction plant.
  • the top product of T3 can, after further cooling, be fed via line 13, possibly via an expansion valve d, to a further separation column T5 (hydrogen separation column), alternatively to one or more separators, in order to To separate helium and possibly other noble gases from hydrogen.
  • the top product of T5 can then be fed to an inert gas liquefaction plant (B8), preferably a helium liquefaction plant, and the bottom product of T5 can be further processed to form liquid hydrogen (B7).
  • the liquid products are then stored in vacuum-insulated special tanks.
  • the process is supplied with cold by means of a coolant or coolant mixture and by heating the products in E1.
  • a coolant or coolant mixture and by heating the products in E1.
  • the figure shows a nitrogen expander cycle as an example; alternatively, a nitrogen-methane expander cycle or a mixture cycle can also be optimal.
  • Several identical or different refrigeration circuits can also be used.
  • the low-pressure refrigerant flow in line 21 is fed to a single-stage or multi-stage circuit compression, after which the final pressure of the expander circuit is adjusted via the compressors coupled to the expander(s).
  • the high-pressure circulatory flow cooled against air or water is then pre-cooled via line 22 in E1.
  • a partial flow (line 23) is drawn off and expanded in expander X1 to provide cold in E1 24.
  • the high-pressure main flow is further cooled in E1 25 and finally expanded in X2 26, heated in E1, mixed with the flow to X1, further heated in E1 and fed to the compression cycle 21 .
  • the refrigerant component nitrogen can preferably be metered in in the cold part of the circuit 27, but also after the HP nitrogen (B5) has been heated up.
  • a nitrogen-methane expander circuit can also be used, with the methane content of the refrigerant preferably being obtained from the methane product (B4) or the bottom product of T2.
  • the second expander compressor X2-C2 can possibly be omitted and replaced by a throttle valve g.
  • the heat exchangers that provide the top cold for the various rectification columns can either be designed as plate exchangers, coiled heat exchangers or TEMA exchangers and arranged in or above the respective rectification column, with an arrangement above the rectification columns being a return pump obsolete.
  • the contamination of the respective top products can be kept within narrow limits, e.g. the methane content in the fraction drawn off via line 9 can be almost arbitrary, namely between approx. 1 ppm to a few [% by volume, preferably less than 2% by volume, particularly preferably less than 1% by volume.
  • the method according to the invention for obtaining valuable materials from a hydrogen-rich feed gas in particular a hydrogen-rich natural gas, can be used in an advantageous manner with hydrogen contents of 50% by volume or more.
  • hydrogen contents 50% by volume or more.
  • the hydrogen product and the methane product are not liquefied, even comparatively high nitrogen and methane contents in the feed fraction only have a minor effect on the total energy requirement of the process according to the invention, since part of the cold caused by heating the products hydrogen, nitrogen and methane in E1 is recovered.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Hydrogen, Water And Hydrids (AREA)

Abstract

L'invention concerne un procédé cryogène pour la récupération de matière valorisable, notamment d'hydrogène, à partir d'un gaz d'alimentation riche en hydrogène, en particulier de gaz naturel riche en hydrogène, comprenant les étapes suivantes consistant à : séparer dans une première colonne de séparation (T1) des hydrocarbures comportant au moins deux atomes de carbone ; séparer du méthane dans une seconde colonne de séparation (T2) ; et séparer de l'azote dans une troisième colonne de séparation (T3), le gaz d'alimentation riche en hydrogène, après avoir subi un éventuel prélavage (R), alimentant les colonnes de séparation T1 à T3 dans l'ordre des étapes a) à c), et les colonnes de séparation étant le siège d'une séparation en une fraction liquide, le résidu de distillation, et une fraction gazeuse, le produit de tête. Dans le procédé cryogène selon l'invention, l'apport de froid est réalisé de préférence au moins en partie par l'intermédiaire d'un ou plusieurs circuits de refroidissement.
EP21823483.9A 2020-11-23 2021-11-22 Procédé cryogène pour la récupération de matière valorisable à partir d'un gaz d'alimentation riche en matière valorisable Pending EP4244559A2 (fr)

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DE102020130946.5A DE102020130946B4 (de) 2020-11-23 2020-11-23 Kryogenes Verfahren zur Wertstoffgewinnung aus einem wasserstoffreichen Einsatzgas
PCT/EP2021/082545 WO2022106699A2 (fr) 2020-11-23 2021-11-22 Procédé cryogène pour la récupération de matière valorisable à partir d'un gaz d'alimentation riche en matière valorisable

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CN115790076B (zh) * 2023-02-08 2023-05-23 杭氧集团股份有限公司 一种回收烟道气中二氧化碳和氮气的装置及方法
CN118310251B (zh) * 2024-05-06 2025-05-27 杭州中泰深冷技术股份有限公司 丙烷脱氢制丙烯产物深冷分离与氢液化联产系统及方法

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WO2022106699A3 (fr) 2022-09-29
WO2022106699A4 (fr) 2022-11-17
DE102020130946B4 (de) 2023-02-02
US20240019206A1 (en) 2024-01-18
WO2022106699A2 (fr) 2022-05-27
CN116601447A (zh) 2023-08-15
ZA202306101B (en) 2025-04-30
CA3199710A1 (fr) 2022-05-27
DE102020130946A1 (de) 2022-05-25

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