WO2025073664A1 - Prétraitement de gaz naturel brut riche en alcanes en c2-c6 ou de gaz de dégagement industriel - Google Patents

Prétraitement de gaz naturel brut riche en alcanes en c2-c6 ou de gaz de dégagement industriel Download PDF

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Publication number
WO2025073664A1
WO2025073664A1 PCT/EP2024/077545 EP2024077545W WO2025073664A1 WO 2025073664 A1 WO2025073664 A1 WO 2025073664A1 EP 2024077545 W EP2024077545 W EP 2024077545W WO 2025073664 A1 WO2025073664 A1 WO 2025073664A1
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Prior art keywords
alkanes
gas
natural gas
rich
vol
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Inventor
Dieter Flick
William DALOZ
Jens Peter JOHANNSEN
Daniela Rieck
Johannes BODE
Joern Alexander JUDITH
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BASF SE
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BASF SE
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Classifications

    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen; Reversible storage of hydrogen
    • C01B3/02—Production of hydrogen; Production of gaseous mixtures containing hydrogen
    • C01B3/22—Production of hydrogen; Production of gaseous mixtures containing hydrogen by decomposition of gaseous or liquid organic compounds
    • C01B3/24—Production of hydrogen; Production of gaseous mixtures containing hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen; Reversible storage of hydrogen
    • C01B3/02—Production of hydrogen; Production of gaseous mixtures containing hydrogen
    • C01B3/22—Production of hydrogen; Production of gaseous mixtures containing hydrogen by decomposition of gaseous or liquid organic compounds
    • C01B3/24—Production of hydrogen; Production of gaseous mixtures containing hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons
    • C01B3/28—Production of hydrogen; Production of gaseous mixtures containing hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons using moving solid particles, e.g. fluidised bed technique
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/08—Methods of heating or cooling
    • C01B2203/0805—Methods of heating the process for making hydrogen or synthesis gas
    • C01B2203/085—Methods of heating the process for making hydrogen or synthesis gas by electric heating
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/08—Methods of heating or cooling
    • C01B2203/0805—Methods of heating the process for making hydrogen or synthesis gas
    • C01B2203/0861—Methods of heating the process for making hydrogen or synthesis gas by plasma
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/08—Methods of heating or cooling
    • C01B2203/0872—Methods of cooling
    • C01B2203/0883—Methods of cooling by indirect heat exchange
    • 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
    • C10L2290/02—Combustion or pyrolysis
    • 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
    • C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel

Definitions

  • US 2016/340596 discloses a method for providing pipeline quality natural gas from raw natural gas feed stream by separating and recovering natural gas liquids with an adsorption process.
  • the deposition of carbon can result in coke deposition on reactor equipment like feed inlet and on the reactor wall or can result in agglomeration of carrier bed particles.
  • Several negative aspects are associated with this agglomeration process.
  • stronger agglomerated beds require a more complex, slower procedure to remove the carrier bed.
  • moving bed reactors a higher level of agglomeration between carrier particles can lead to a blockage of the solid flow.
  • large agglomerates may no longer be fluidized, thus disrupting the fluidization behavior of the bed ending with a collapse of the fluidized bed.
  • the decomposition might already start in or near the inlet feed resulting in a rapid block of the inlet feed equipment.
  • C2-C6 alkanes rich natural gas C2-C6 alkanes rich industry off gas from other industry processes like petroleum refineries could be used as a feedstock for the pyrolysis unit.
  • such refinery off gas liquified petroleum gas, as the following content of C2-C4 alkanes: 0 to 5 Vol.-% ethane, 25 to 45 Vol.-% propane, 50 to 70 Vol.-% butane and trace N2, CO, and H2S.
  • the reactor is operated preferably at 800 °C - 1800 °C and more preferably from 1200 °C - 1600 °C. Beside the temperature, the process is preferably be controlled by diluting the C2-C6 alkanes-rich natural gas feed with hydrogen to a volume ratio of preferably H2/C1 + of 0.1 to 25, even more preferably 0.5 to 25, in particular 1 to 25, even more preferably 2 to 25.
  • C1 + stands for all hydrocarbons.
  • the H2/C1 + ratio is a H2/(C1-C6) ratio.
  • the "gaseous product stream” preferably contains 50 to 99.9 Vol.-% hydrogen, preferably 70 to 99.9 Vol.-% hydrogen, more preferably 95 to 99.9 Vol.-% hydrogen and the remainder methane and residual, reduced C2-C4 alkanes.
  • the reactor is operated preferably at 800 °C - 1800 °C and more preferably from 1200 °C - 1600 °C.
  • the process is preferably be controlled by diluting the C2-C4 alkanes -rich natural gas feed with hydrogen to a volume ratio of preferably H2/C1 + of 0.1 to 25, even more preferably 0.5 to 25, in particular 1 to 25, even more preferably 2 to 25.
  • C1+ stands for all hydrocarbons.
  • the H2/C1 + ratio is a H2/(C1-C6) ratio.
  • the gaseous product stream containing mainly hydrogen could be used in the gas streams of the gas welling site and/or to generate CO2-free electricity/power for the gas welling site or other processes close by.
  • the gaseous product stream can still contain carbon oxide and inert gases, e.g. nitrogen.
  • inert gases e.g. nitrogen.
  • Corresponding hydrogen recovery apparatuses are common knowledge to the person skilled in the art, for example pressure swing adsorption or permeation.
  • no extraction of unreacted hydrocarbons is needed e.g. via hydrogen recovery apparatuses, if the gaseous product stream is fed into a natural gas grid.
  • the hydrogen content is preferably adjusted so that the proportion of hydrogen which is permissible for introduction into the gas grid is adhered to.
  • An exemplary range is 5- 15 vol.-% hydrogen.
  • the existing infrastructure is used. If the gaseous product stream exceeds the proportion of hydrogen which is permissible for introduction into a natural gas grid, the stream is to be fed into a gas grid designed for the distribution of hydrogen-rich gases.
  • the gaseous product stream could be mixed/blended with C2-C6 alkanes rich raw natural gas and/or other natural gas before feeding this blended natural gas mixture into a natural gas grid in such an amount which is permissible in view of the allowed heating values and hydrogen content (see #2b of Figure 2).
  • the heat for the thermal pyrolysis reaction is supplied by pulsed combustion (see for example WC2020118417 and US20220185664).
  • a feedstock containing hydrocarbon
  • a combustible gas containing hydrocarbons and oxidants
  • the reaction in the combustion chamber takes place when the gas mixture is heated up to 1350K and a pressure of over 20 bar is reached. Products leaving the reactor will be separated into gas and solid carbon for further processing.
  • the pyrolysis processes using molten metals or molten metal salts use the heat from the melt for pyrolysis.
  • metals can be selected that have a catalytic effect, so that pyrolysis can take place at relatively low temperatures of about 800 - 1200 °C.
  • the C2-C4 alkanes rich, especially ethane rich, natural gas or off-gas is fed into the molten metal; the bubbles formed in the process rise upwards in the reactor, whereby the hydrocarbons decompose and form mainly methane, hydrogen and solid carbon.
  • the hydrocarbon decomposition is preferably conducted in a moving or fixed bed reactor, wherein the bed contains as substrates preferably carbon materials, metals, ceramics, and a mixture thereof, preferably at temperatures ranging from 500 to 2000°C, preferably ranging from 1000 to 1600°C, even more preferably ranging from 1200 to 1500°C, and at pressures ranging from 1 to 100 bar, preferably from 5 to 50 bar.
  • substrates preferably carbon materials, metals, ceramics, and a mixture thereof, preferably at temperatures ranging from 500 to 2000°C, preferably ranging from 1000 to 1600°C, even more preferably ranging from 1200 to 1500°C, and at pressures ranging from 1 to 100 bar, preferably from 5 to 50 bar.
  • the decomposition process is preferably heated electrically, even more preferably by resistive heating (Joule heating) of the substrate material as described for example in US 2982622, WO 2019/145279 and WO 2020/200522.
  • the gas residence time in the reactor is advantageously between 0.5 and 50 s, preferably between 1 and 20 s.
  • the residence time of the substrate is preferably between 0.5 and 15 hours, preferably between 1 and 10 hours and more preferably between 2 and 8 hours.
  • the substrates are carbonaceous materials that are macro-structured carbonaceous materials, wherein the porosity of the carbonaceous material is in the range of 30 to 70 vol.-% and the carbonaceous material contains of a carbon content of 98 Vol.-% to 100 Vol.-%, preferably 99 Vol.-% to 100 Vol.-%, even more preferably 99.5 Vol.- % to 100 Vol.-% and a content of alkaline-earth metals, transition metals and metalloids of 0 and 2 Vol.-%, preferably 0 to 1 Vol.-%, even more preferably 0 to 0.5 Vol.-%, in relation to the total mass of solid carbonaceous material (see WO 2023/057242).
  • the ash content of the granular pyrolytic carbon composition is in the range of 0.001 to 1 weight-% of the composition, preferably 0.01 to 0.2 weight-%.
  • the carbon content of the granular pyrolytic carbon composition is in the range of 98 to 100 weight-%, more preferably 99.5 to 100 weight-%, even more 99.75 to 100 weight-%, even more 99.9 to 100 weight-%.
  • the particle size of the granular pyrolytic carbon directly resulting of the decomposition of gaseous hydrocarbons - without any agglomeration step - is in the range of 0.3 mm (d10) to 8 mm (d90), preferably 0.5 mm (d10) to 5 mm (d90), more preferably 1 mm (d10) to 4 mm (d90).
  • the specific surface area of the granular pyrolytic carbon measured by Hg porosimetry is in the range of 0.001 to 10 m2/g, preferably 0.001 to 5 m2/g, even more preferably 0.05 to 2 m2/g.
  • the reactor for carrying out the methane decomposition in which methane, hydrogen and granular pyrolytic carbon are produced from C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas, comprises:
  • C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas in the reaction zone can be heated to a reaction temperature to produce methane, hydrogen and granular pyrolytic carbon
  • the reactor interior also comprises a first heat integration zone in which heat from methane and hydrogen produced in the reaction zone can be transferred to solid substrates of the reactor gravity driven moving bed which are to be guided into the reaction zone, and wherein the reactor interior also comprises a second heat integration zone in which heat from solid substrates of the reactor gravity driven moving bed coming from the reaction zone can be transferred to C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas in order to preheat C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas, wherein said reaction zone is arranged between said pair of first and second electrodes and said first heat integration zone is arranged above said first electrode and said second heat integration zone is arranged below said second electrode.
  • C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas is introduced into the second heat integration zone and from there into the reaction zone, wherein C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas in the second heat integration zone is heated against solid substrates coming from the reaction zone, wherein the solid substrates are cooled, and wherein the C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas is contacted with the heated solid substrates in the reaction zone, wherein heat from the heated solid substrates is transferred to C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas in order to heat C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas in the reaction zone, wherein C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas is decomposed
  • - withdrawn hydrogen is preferably at least partly recycled and introduced into the reactor.
  • the deposition rate for the decomposition of the C2 to C6 alkanes being a reactive feedstock is to be kept in a range of preferably 0.1 to 20 wt.-%, more preferably 1 to 15 %, more preferably 2 to 12 %, even more preferably 3 to 10 wt.-%, even more preferably 4 to 8 wt.-%.
  • the carbon deposition rate is preferably also be controlled by the conversion rate that is preferably 5 to 85 %, more preferably 10 to 80 %, more preferably 25 to 80 %, even more preferably 50 to 80 % (based on the hydrocarbons in the feed stream).
  • an internal direct recycle of the hydrogen-containing gaseous product stream is used to dilute the feed stream and control the H2/C1+ volume ratio, that means, a portion of the raw gaseous product stream is recycled without any purification steps (see Figure 4).
  • Said recycled gaseous product stream may or may not be cooled, heated and/or compressed.
  • the gaseous product stream leaving the reaction chamber preferably enters a distribution unit.
  • This distribution unit typically includes a valve, a flow meter, and a meter to determine the H2 concentration.
  • vol-% to 90 vol-% of the gaseous product stream is separated in the distribution unit and recycled to the reaction chamber, more preferably 20 vol -% to 85 vol %, more preferably 30 vol- % to 85 vol -%, even more preferably 40 vol -% to 80 vol -%, even more preferably 50 vol -% to 80 vol -%.
  • the vol-% of the gaseous product stream taken for the internal direct recycle is preferably adjusted to a volume ratio H2/C1 + of the total reactor feed stream ranging from 0.1 to 25, more preferably from 0.5 to 10, even more preferably from 1 to 8.
  • the ratio of the volume of the internally recycled hydrogen-containing gaseous product stream to the volume of the external feed stream is between 0.1 to 20, more preferably between 0.3 and 8, even more preferably between 0.8 and 6.
  • the total feed of the pyrolysis process has a fixed H2/C+ feed molar, the operation point. The operating point enables an optimal heat integration and is dependent on the hydrocarbon concentration, the substrate used and the deposition rate of the solid carbon.
  • a dedicated amount of hydrogen could be recycled or added, preferably recycled as mentioned above and shown in the Figures 4 and 5.
  • the operation point of the pyrolysis unit is preferably set between 50 to 99 vol.%, more preferably between 70 and 99 vol.-% hydrogen and 1 to 50 vol .-%, more preferably 1 and 30 vol.-% hydrocarbons related to the total volume of the total feed. Due to the fact that the total feed concentration of the reactor could be controlled by a hydrogen recycle, there is a broad and fluctuating range for the concentration of hydrocarbons in the C2-C6 alkanes rich natural gas and/or C2-C6 alkanes rich industry off-gas applicable.
  • Fig 5 shows the block diagram of a general embodiment of the process of the invention in which also a part of the off gas from the hydrogen recovery is recycled to the pyrolysis unit.
  • Table3 Process conditions natural gas pyrolysis in a moving bed reactor
  • results show much faster species decomposition when using C2H6 or C3H8 as part of the feed gas (compared to pure CH4) and thus indicate a higher risk for clogging, e.g. inside pre-heating equipment necessary for the operation of a fluidized bed reactor.
  • results show notable formation of soot precursors in less than 1 sec (10 3 ms) for C2H6 and C3H8 mixtures and thus indicate a higher risk for soot formation and hereafter blocking.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

La présente invention concerne un processus de traitement d'un gaz naturel riche en alcanes en C2-C6 ayant une teneur en alcane en C2-C6 de 2,5 à 30 % du volume total du gaz naturel brut ou d'un gaz de dégagement industriel riche en alcanes en C2-C6 ayant une teneur en alcane en C2-C6 de 10 à 80 % du volume total du gaz de dégagement industriel pour obtenir du gaz naturel de pipeline de qualité ou de l'hydrogène de pipeline de qualité, (i) le gaz naturel riche en alcanes en C2-C6 et/ou le gaz de dégagement industriel riche en alcanes en C2-C6 étant introduits par le fond d'un réacteur à lit mobile ayant une température de 10 à 200 °C, et des substrats ayant une taille de particule de 0,3 à 8 mm sont introduits par le haut dudit réacteur à lit mobile ayant une température de 10 à 200 °C, (ii) le gaz naturel riche en alcanes en C2-C6 et/ou le gaz de dégagement industriel riche en alcanes en C2-C6 étant pyrolysés dans ledit réacteur à lit mobile en un flux de produit gazeux contenant au moins du méthane et/ou de l'hydrogène et en carbone solide, (iii) le carbone solide étant séparé de ce flux de produit gazeux et (iv) le flux de produit gazeux étant introduit dans un réseau de gaz naturel et/ou dans un réseau d'hydrogène ou le flux de produit gazeux étant directement utilisé matériellement ou énergétiquement.
PCT/EP2024/077545 2023-10-06 2024-10-01 Prétraitement de gaz naturel brut riche en alcanes en c2-c6 ou de gaz de dégagement industriel Pending WO2025073664A1 (fr)

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EP23202057 2023-10-06

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Citations (17)

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US2982622A (en) 1958-09-02 1961-05-02 Exxon Research Engineering Co Hydrocarbon conversion process
US20020007594A1 (en) 2000-04-05 2002-01-24 Muradov Nazim Z. Thermocatalytic process for CO2-free production of hydrogen and carbon from hydrocarbons
WO2011029144A1 (fr) 2009-09-10 2011-03-17 The University Of Western Australia Procede de production d'hydrogene a partir d'hydrocarbures
WO2013004398A2 (fr) 2011-07-05 2013-01-10 Linde Aktiengesellschaft Procédé de production parallèle d'hydrogène et de produits à base de carbone
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WO2011029144A1 (fr) 2009-09-10 2011-03-17 The University Of Western Australia Procede de production d'hydrogene a partir d'hydrocarbures
WO2013004398A2 (fr) 2011-07-05 2013-01-10 Linde Aktiengesellschaft Procédé de production parallèle d'hydrogène et de produits à base de carbone
WO2015116797A1 (fr) 2014-01-30 2015-08-06 Monolith Materials, Inc. Intégration d'un procédé au plasma et à l'hydrogène dans une centrale électrique à cycle combiné et reformeurs à vapeur
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WO2021183959A1 (fr) 2020-03-13 2021-09-16 C-Zero Llc Procédés d'élimination de carbone pneumatique
US20220185664A1 (en) 2020-12-15 2022-06-16 Ekona Power Inc. Methods of producing one or more products using a feedstock gas reactor
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