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AU2016304194B2 - Method for separating carbon dioxide from a hydrocarbon-rich fraction - Google Patents
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AU2016304194B2 - Method for separating carbon dioxide from a hydrocarbon-rich fraction - Google Patents

Method for separating carbon dioxide from a hydrocarbon-rich fraction Download PDF

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Publication number
AU2016304194B2
AU2016304194B2 AU2016304194A AU2016304194A AU2016304194B2 AU 2016304194 B2 AU2016304194 B2 AU 2016304194B2 AU 2016304194 A AU2016304194 A AU 2016304194A AU 2016304194 A AU2016304194 A AU 2016304194A AU 2016304194 B2 AU2016304194 B2 AU 2016304194B2
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rich
gas fraction
fraction
pressure
hydrocarbon
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AU2016304194A1 (en
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Heinz Bauer
Claudia Gollwitzer
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Linde GmbH
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Linde GmbH
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
    • F25J3/0209—Natural gas or substitute natural gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/229—Integrated processes (Diffusion and at least one other process, e.g. adsorption, absorption)
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas
    • C10L3/101—Removal of contaminants
    • C10L3/102—Removal of contaminants of acid contaminants
    • C10L3/104—Carbon dioxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0233—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of CnHm with 1 carbon atom or more
    • 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
    • F25J3/0266—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 dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/24—Hydrocarbons
    • B01D2256/245—Methane
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/65—Employing advanced heat integration, e.g. Pinch technology
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/06—Heat exchange, direct or indirect
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/46—Compressors or pumps
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/48—Expanders, e.g. throttles or flash tanks
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
    • C10L2290/545—Washing, scrubbing, stripping, scavenging for separating fractions, components or impurities during preparation or upgrading of a fuel
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
    • C10L2290/548—Membrane- or permeation-treatment for separating fractions, components or impurities during preparation or upgrading of a fuel
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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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/02—Processes or apparatus using separation by rectification in a single 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
    • F25J2200/40—Features relating to the provision of boil-up in the bottom of a 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
    • 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
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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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    • 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
    • F25J2205/80—Processes or apparatus using other separation and/or other processing means using membrane, i.e. including a permeation step
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/04—Mixing or blending of fluids with the feed stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/06—Splitting of the feed stream, e.g. for treating or cooling in different ways
    • 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
    • F25J2215/04—Recovery of liquid products
    • 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
    • F25J2220/80—Separating impurities from carbon dioxide, e.g. H2O or water-soluble contaminants
    • F25J2220/82—Separating low boiling, i.e. more volatile components, e.g. He, H2, CO, Air gases, CH4
    • 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
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    • F25J2230/04—Compressor cooling arrangement, e.g. inter- or after-stage cooling or condensate removal
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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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
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    • F25J2270/00—Refrigeration techniques used
    • F25J2270/04—Internal refrigeration with work-producing gas expansion loop
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    • F25J2270/12—External refrigeration with liquid vaporising loop
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    • F25J2270/00—Refrigeration techniques used
    • F25J2270/60—Closed external refrigeration cycle with single component refrigerant [SCR], e.g. C1-, C2- or C3-hydrocarbons
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    • F25J2270/00—Refrigeration techniques used
    • F25J2270/66—Closed external refrigeration cycle with multi component refrigerant [MCR], e.g. mixture of hydrocarbons
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    • F25J2270/00—Refrigeration techniques used
    • F25J2270/80—Quasi-closed internal or closed external carbon dioxide refrigeration cycle
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    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

The invention relates to a method for separating a CO

Description

Description
Method for separating carbon dioxide from a hydrocarbon-rich fraction
The invention relates to a method for separating off a C0 2-rich liquid fraction from a hydrocarbon-rich, C02-containing gas fraction.
Natural gas and petroleum-associated gases contain acid gases - substantially C02, in addition H 2S and other sulphur compounds, such as COS and mercaptans - in differing concentrations; these acid gases are usually separated off by scrubbing (e.g. amine scrubbers) at ambient temperature. From a C02 concentration of about 10 mol%, this procedure becomes uneconomic, since the circulating amount of scrubbing medium and the energy requirement for the scrubbing medium regeneration constantly increase.
Therefore, for some time membranes, preferably polymer membranes, are being used to decrease the C02 content of the feed gas upstream of an amine scrubber to about 2 to 10 mol%, in such a manner that it can be operated optimally again. Membranes alone, however, are unsuitable to achieve high purities and simultaneously high yields. The combination of a membrane with a low-temperature fractionation is suitable in principle to solve this problem.
Any discussion of the prior art throughout the specification should in no way be considered as an admission that such prior art is widely known or forms part of common general knowledge in the field.
US patent 5,414,190 discloses a method procedure in which a membrane is connected upstream of a low-temperature fractionation of the retentate. A further workup of the C0 2-rich permeate, e.g. to increase the hydrocarbon yield, however, is not disclosed. On account of the hydrocarbon content of the C0 2-rich permeate, in this case, however, unacceptable hydrocarbon losses with reference to the crude gas, occur.
US patent application 2005/0092594 describes a method in which C0 2-rich natural gas is preseparated by rectification and is subsequently set to a low C02 content by means of a membrane. However, this method can only be carried out from about 25 mol%
C02, since at lower C02 contents the proposed low-temperature fractionation is without effect, since C02 does not condense under the disclosed conditions and therefore cannot be separated off via the sump. Both of the previously described methods are, in addition, unable to provide the C02 that is separated off in the liquid state and in the desired purity.
It is an object of the present invention to overcome or ameliorate at least one of the disadvantages of the prior art, or to provide a useful alternative.
According to the first aspect of the present invention, there is provided a method for separating off a C0 2-rich liquid fraction from a hydrocarbon-rich C02-containing gas fraction, wherein a) the hydrocarbon-rich C02-containing gas fraction is separated by permeation into a C0 2-weak gas fraction and a C0 2-rich gas fraction, b) the C0 2-rich gas fraction is compressed to a pressure which is at least 10% above the critical pressure of the C0 2-rich gas fraction, c) the compressed C0 2-rich gas fraction is cooled and expanded, d) wherein the C0 2-rich gas fraction is cooled to a temperature at which, after expansion thereof, the formation of a solid C0 2-rich phase is avoided, e) the expanded C0 2-rich fraction is separated by means of a stripping process into a C0 2-depleted gas fraction and a C0 2-rich liquid fraction, f) the C0 2-depleted gas fraction is fed to the hydrocarbon-rich C02-containing gas fraction that is to be separated by permeation, and g) the cooling of the compressed C0 2-rich gas fraction proceeds against an open expander circuit, wherein a substream of the C0 2-rich gas fraction is used as coolant.
Further advantageous embodiments of the method according to the invention for separating off a C0 2-rich liquid fraction from a hydrocarbon-rich, C02-containing gas fraction which are subjects of the dependent claims wherein: - the stripping process is operated in such a manner that the C0 2-rich liquid fraction has a C02 content of at least 98 mol%, preferably at least 99.5 mol%,
- the hydrocarbon-rich C02-containing gas fraction contains between 10 and 85 mol% C02, preferably between 25 and 60 mol% C02,
- the C0 2-weak gas fraction contains a maximum of 15 mol% C02, preferably a maximum of 10 mol% C02,
- the membrane used for the separation by permeation (method step a) has a selectivity between C02 and CH 4 of at least 2, preferably at least 3,
- in the separation by permeation (method step a), the pressure on the permeate side is lower than the pressure on the feed side by the factor 4 to 10, preferably 5 to 8,
- where the compression of the C0 2-rich gas fraction proceeds at least in a two stage manner and after each intermediate compressor stage an intercooling of the compressed C0 2-rich gas fraction proceeds, the pressure of the stripping process is selected in such a manner that the sump temperature is lower by at least 10°C, preferably at least 15°C, than the process temperature at which the intercooling of the C0 2-rich gas fraction is achievable,
- the pressure of the stripping process is between 30 bar and 60 bar, and/or
- the cooling of the compressed C02-rich gas fraction proceeds against a closed expander circuit.
According to a second aspect of the present invention, there is provided a C0 2-rich liquid fraction separated off from a hydrocarbon-rich C02-containing gas fraction using the method described herein.
According to the invention, the hydrocarbon-rich, C02-containing gas fraction that has a C02 content between 10 and 85 mol% and that is present at a pressure of 30 to 70 bar, preferably 40 to 60 bar, where necessary, is first fed to a pretreatment in which C5 hydrocarbons and water are separated off. These components can if necessary be delivered together with the retentate that is still to be described. The hydrocarbon-rich gas fraction that is optionally pretreated in such a manner is separated by permeation into a C0 2-weak gas fraction (retentate) and a C0 2-rich gas fraction (permeate). This separation preferably proceeds by means of a polymer membrane. Said polymer membrane advantageously has a selectivity between C02 and CH 4 of at least 2, preferably at least 3. In addition, the pressure on the permeate side is lower by the factor 4 to 10, preferably 5 to 8, than the pressure on the feed side. The selectivity a is taken to mean the ratio of the molar concentrations of C02 and CH 4 in the permeate stream (y) and in the feed (x) to the membrane:
CO2 /CH4
The C0 2-rich gas fraction is then compressed to a pressure which is at least 10% above the critical pressure of this C0 2-rich gas fraction. Generally, the C0 2-rich gas fraction is compressed in two or more stages. The (intermediately) compressed C02 rich gas fraction is preferably intercooled or post-cooled against cooling water and/or air. The compressed C0 2-rich gas fraction is cooled by means of a suitable refrigeration apparatus and then expanded. In this case, it is cooled to a temperature at which, after the expansion, the formation of a solid C0 2-rich phase can be reliably be avoided; generally, cooling proceeds to a temperature which is at least 50C, preferably at least 1O0C, above the melting point of carbon dioxide.
The expanded C0 2-rich fraction is separated by means of a stripping process into a C02-depleted gas fraction and a C0 2-rich liquid fraction. Since the liquid proportion of the expanded C0 2-rich fraction is generally too rich in hydrocarbons, in particular methane, to comply with the requirements of C02 purity, the C0 2-rich fraction fed to the stripping process or the stripping column is purified by removing methane by boiling until the C0 2-rich liquid fraction taken off from the sump of the stripping column - which fraction is the product stream - has the desired composition. Advantageously, this C0 2-rich liquid fraction usually has a C02 content of at least 98 mol%, preferably at least 99.5 mol%.
Where the C0 2-rich gas fraction is compressed in at least two stages, and after each intermediate compressor stage and intercooling of the compressed C0 2-rich gas fraction proceeds, advantageously the pressure of the stripping process is selected in such a manner that the sump temperature is lower by at least 10°C, preferably at least 150C, than the process temperature which is achievable in the intercooling of the C02 rich gas fraction; generally, therefore, a pressure between 30 and 60 bar is selected.
By means of this method procedure, the cooling capacity of the methane vaporizing in the stripping column is at least partially utilized in order to lower the intake temperatures of the compressor stages and therefore the energy consumptions thereof.
The C0 2-depleted gas fraction obtained at the top of the stripping column is fed to the hydrocarbon-rich gas fraction that is to be separated by permeation. For this purpose, the C0 2-depleted gas fraction is warmed in advance to ambient temperature. Usually, no additional compression is required before the admixture.
The method according to the invention for separating off a C0 2-rich liquid fraction from a hydrocarbon-rich C02-containing gas fraction, and also further embodiments thereof will be described in more detail hereinafter with reference to the exemplary embodiments shown in Figures 1 to 4.
The hydrocarbon-rich C02-containing gas fraction 1 that has a C02 content between 10 and 85 mol% and is usually present at a pressure from 30 to 70 bar, is fed to a pretreatment P, which is shown merely as a black box, in which C5. hydrocarbons and/or water are separated off. Where separation of C5. hydrocarbons and/or water is not required, this pretreatment P can be dispensed with. The optionally pretreated hydrocarbon-rich gas fraction 1' is then separated by permeation M into a C0 2-weak gas fraction 2 and a C0 2-rich gas fraction 3. This separation preferably proceeds by means of a polymer membrane. The C0 2-rich gas fraction 3 is compressed in the compressor stages C1, C2 and C3 to a pressure which is at least 10% above the critical pressure of the C0 2-rich gas fraction. The intercooling of the C0 2-rich gas fraction 4 and 5 compressed to intermediate pressures proceeds in the heat exchangers El and E3 against cooling water or air. The C0 2-rich gas fraction 6 that is compressed in the compressor C3 to the desired final pressure is post-cooled in the heat exchanger E5 against cooling water or air. The compressed C0 2-rich gas fraction 6 is cooled in the heat exchanger E6 against a suitable refrigeration facility R which is merely shown as a black box in Figure 1; for this purpose, the refrigeration facility R is coupled to the heat exchanger E6 via the cold circuit 12. Subsequently, the cooled C0 2-rich gas fraction 6 is expanded in the valve V1 and fed to the top of the stripping column T1. In this case, the compressed C0 2-rich gas fraction 6 is cooled in the heat exchanger E6 to a temperature at which the formation of a solid C0 2-rich phase after the expansion in valve V1 can reliably be prevented. For this reason, cooling proceeds to a temperature which is at least 5°C, preferably at least 10°C, above the melting point of carbon dioxide.
The C0 2-rich fraction fed to the stripping column T1 is separated into a C0 2-depleted gas fraction 7 and a C0 2-rich liquid fraction 8. The latter is delivered via the control valve V2. Since the liquid proportion of the expanded C0 2-rich fraction is generally too rich in hydrocarbons, in particular methane, in order to meet the requirements of C02 purity of the C0 2-rich liquid fraction 8, the C0 2-rich fraction that is fed to the stripping column is purified by removal of methane by boiling to the extent that the C02 liquid fraction 8 has the desired purity, that is to say has a C02 content of at least 98 mol%, preferably at least 99.5 mol%. For this purpose, a substream 9 that is taken off from the C0 2-rich liquid fraction from the sump of the stripping column T1 is taken off and divided into two substreams 9 and 9'. Substream 9 is warmed in the heat exchangers E2 and E4 against the C0 2-rich gas fraction which is compressed and is to be cooled, at least partially vaporized and together with the substream 9' that is warmed in the refrigeration plant R and is at least in part vaporized is fed to the stripping column T1 as stripping vapour.
Advantageously, the pressure within the stripping column T1 is selected in such a manner that the sump temperature thereof is at least 10C, preferably at least 15°C, below the process temperature which is achievable in the intercooling of the compressed C0 2-rich gas fraction in the heat exchangers Ei and E3. Therefore, the pressure within the stripping column T1 is generally 30 to 60 bar. By means of this method procedure, the cooling capacity of the methane vaporized in the stripping column T1 can be utilized at least in part to lower the intake temperatures of the compressor stages C2 and C3 and thereby the energy consumptions thereof.
The C0 2-depleted gas fraction 7 obtained at the top of the stripping column is warmed in the heat exchanger E6 (to ambient temperature) and fed to the hydrocarbon-rich gas fraction 1' that is to be separated by permeation.
In Figures 2 to 4, now three different embodiments are shown of the refrigeration facility or refrigeration provision R which is merely shown as a black box in Figure 1, which serves for cooling the compressed C0 2-rich gas fraction 6.
Where a comparatively simple operation and high flexibility have priority over a low energy consumption - this is the case, for example in the case of offshore plants - an open expander circuit is to be preferred, as explained with reference to the exemplary embodiment shown in Figure 2. In this case, a substream 20 of the C0 2-rich gas fraction 4 which is compressed to an intermediate pressure is taken off downstream of the heat exchanger E2, increased in pressure by an additional compressor C4 and then cooled in the heat exchanger E7 against cooling water or air and in heat exchanger E8 against the substream 9 of the C0 2-rich liquid fraction 8 that is to be vaporized. Subsequently, the cooled substream 21 work-producingly expanded in an expansion turbine X1 that is coupled to the above-described compressor C4; the mechanical power of the expansion turbine X1 is used for driving the compressor C4. This expansion can if necessary also be carried out in a multistage manner, optionally with an intermediate warming. The additional heat exchanger E8 serves analogously to the heat exchangers E2 and E4 to lower the intake temperature of the expansion turbine X1 in an energy saving manner.
The heat-exchanger system E6 shown in Figure 1, in the exemplary embodiment shown in Figure 2, is divided into two parallel-arranged heat exchangers E6 and E6' with the purpose of optimizing what are termed helically coiled heat exchangers. Whereas the C0 2-rich gas fraction 6 that is to be cooled, on account of the comparatively high pressure thereof, is conducted on the tube side, the cold streams 7 and 21 are conducted on the shell side. The substream 22 that is warmed in the heat exchanger E6' and is used as coolant is admixed to the C0 2-rich gas fraction 3 before the compression thereof.
Where high efficiency is more important than simple operation, preferably differing types of closed cold circuits having phase change of the coolant are used. In the exemplary embodiment shown in Figure 3, a comparatively simple mixed cycle is shown in which the coolant circulating therein consists of a mixture of at least two light hydrocarbons of the group C1 to C (methane, ethylene, ethane, propylene, propane, butane and pentane). The coolant 31 compressed in the compressor C4 is completely condensed in the heat exchangers E7 and E8 against cooling water or air, or against the substream 9 of the C0 2-rich liquid fraction 8. The container D1 serves for storage of liquid coolant in order to permit differing operating states. The coolant mixture 32 taken off from the container D1 is subcooled in the heat exchanger E6', expanded in the expansion valve V3, completely vaporized at a comparatively low pressure on the shell side of the heat exchanger E6', which is preferably a helically coiled heat exchanger, and then fed back to the compressor C4.
By choosing a closed mixed circuit, as is shown by way of example in Figure 3, in comparison with an open expander circuit, as is shown in Figure 2, 20 to 40% of the power can be saved. However, the provision of the mixed circuit components and the proper use thereof increases the expenditure considerably.
In the exemplary embodiment shown in Figure 4, the compressed C0 2-rich gas fraction 6 is cooled by means of a pure coolant. In order to keep the energy similarly favourable as in the mixed circuit described with reference to Figure 3, the coolant that is compressed in the compressor C4 and liquefied in the heat exchangers E7 and E8 is vaporized at at least two pressure stages in the heat exchangers E6' and E6". For this purpose, the coolant 43 that is taken off from the container D1 is first fed via the expansion valve V3 to the heat exchanger E6', a part of the coolant is vaporized therein and fed via line 40 to the intermediate stage of the compressor C4, whereas the residual coolant substream is expanded via the control valve V4 into the heat exchanger E6". The coolant stream 41 vaporized in the heat exchanger E6" is fed to the suction side of the compressor C4. Coolants that come into consideration for such a pure coolant circuit are all substances which can be liquefied at ambient temperature. These include, inter alia, propane, propylene, R22, R134a and, at a low ambient temperature, also ethane and also carbon dioxide.
The method according to the invention for separating off a C0 2-rich liquid fraction from a hydrocarbon-rich C02-containing gas fraction permits liquid C02 to be separated off in technically pure form, that is to say having a C02 content of at least 98 mol%, from a crude gas having a high bandwidth of C02 concentration. In addition, the C02 content of the C0 2-weak gas fraction can be reduced therewith to less than 10 mol%. Furthermore, the hydrocarbon losses via the liquid C02 product fraction may be reduced to less than 2%.

Claims (16)

Claims
1. Method for separating off a C0 2-rich liquid fraction from a hydrocarbon-rich C02 containing gas fraction, wherein a) the hydrocarbon-rich C02-containing gas fraction is separated by permeation into a C0 2-weak gas fraction and a C0 2-rich gas fraction, b) the C0 2-rich gas fraction is compressed to a pressure which is at least 10% above the critical pressure of the C0 2-rich gas fraction, c) the compressed C0 2-rich gas fraction is cooled and expanded, d) wherein the C0 2-rich gas fraction is cooled to a temperature at which, after expansion thereof, the formation of a solid C0 2-rich phase is avoided, e) the expanded C0 2-rich fraction is separated by means of a stripping process into a C0 2-depleted gas fraction and a C 2-rich liquid fraction, f) the C0 2-depleted gas fraction is fed to the hydrocarbon-rich C02-containing gas fraction that is to be separated by permeation, and g) the cooling of the compressed C02-rich gas fraction proceeds against an open expander circuit, wherein a substream of the C02-rich gas fraction is used as coolant.
2. Method according to Claim 1, wherein the stripping process is operated in such a manner that the C0 2-rich liquid fraction has a C02 content of at least 98 mol%.
3. Method according to claim 2, wherein the C0 2-rich liquid fraction has a C02 content of at least 99.5 mol%.
4. Method according to any one of the preceding claims, wherein the hydrocarbon rich C02-containing gas fraction contains between 10 and 85 mol% C02.
5. Method according to claim 4, wherein the hydrocarbon-rich C02-containing gas fraction contains between 25 and 60 mol% C02.
6. Method according to any one of the preceding claims, wherein the C0 2-weak gas fraction contains a maximum of 15 mol% C02.
7. Method according to claim 6, wherein the C02-weak gas fraction contains a maximum of 10 mol% C02.
8. Method according to any one of the preceding claims, wherein the membrane used for the separation by permeation (method step a) has a selectivity between C02 and CH 4 of at least 2.
9. Method according to claim 8, wherein selectivity between C02 and CH 4 is at least 3.
10. Method according to any one of the preceding claims, wherein, in the separation by permeation (method step a), the pressure on the permeate side is lower than the pressure on the feed side by the factor 4 to 10.
11. Method according to claim 10, wherein ), the pressure on the permeate side is lower than the pressure on the feed side by the factor 5 to 8.
12. Method according to any one of the preceding claims, wherein the compression of the C0 2-rich gas fraction proceeds at least in a two-stage manner and after each intermediate compressor stage an intercooling of the compressed C0 2-rich gas fraction proceeds, wherein the pressure of the stripping process is selected in such a manner that the sump temperature is lower by at least 10°C, than the process temperature at which the intercooling of the C0 2-rich gas fraction is achievable.
13. Method according to claim 12, wherein the pressure of the stripping process is selected in such a manner that the sump temperature is lower by at least 15°C.
14. Method according to claims 12 and 13, wherein the pressure of the stripping process is between 30 bar and 60 bar.
15. Method according to any one of the preceding claims, wherein the cooling of the compressed C0 2-rich gas fraction proceeds against a closed expander circuit.
16. A C0 2-rich liquid fraction separated off from a hydrocarbon-rich C02-containing gas fraction using the method according to any one of the preceding claims.
P15C110-DE.doc /IC1737 21.06.2016- Christoph Zahn/bg
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