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WO2024261301A1 - Reformage en boucle chimique d'hydrocarbures - Google Patents

Reformage en boucle chimique d'hydrocarbures Download PDF

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Publication number
WO2024261301A1
WO2024261301A1 PCT/EP2024/067535 EP2024067535W WO2024261301A1 WO 2024261301 A1 WO2024261301 A1 WO 2024261301A1 EP 2024067535 W EP2024067535 W EP 2024067535W WO 2024261301 A1 WO2024261301 A1 WO 2024261301A1
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WO
WIPO (PCT)
Prior art keywords
metal oxide
stochiometric
cycle
gas
production
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Pending
Application number
PCT/EP2024/067535
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English (en)
Inventor
Jonathan Richard SCHEFFE
Caroline Marie HILL
Simon Ackermann
Philipp Furler
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Synhelion SA
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Synhelion SA
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Publication of WO2024261301A1 publication Critical patent/WO2024261301A1/fr
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    • 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
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
    • C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
    • C01B3/36—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using oxygen or mixtures containing oxygen as gasifying agents
    • 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
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
    • C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
    • C01B3/344—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using non-catalytic solid particles
    • 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
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/025—Processes for making hydrogen or synthesis gas containing a partial oxidation step
    • C01B2203/0255—Processes for making hydrogen or synthesis gas containing a partial oxidation step containing a non-catalytic partial oxidation step
    • 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
    • C01B2203/06—Integration with other chemical processes
    • C01B2203/062—Hydrocarbon production, e.g. Fischer-Tropsch process

Definitions

  • the present invention relates to a method for the thermochemical production of a fuel gas such as syngas in a reactor, via a chemical looping process that comprises a process of reforming of a hydrocarbon such as for example methane and a process of splitting carbon dioxide, as well as a device for the production of a method for the thermochemical production of a fuel gas.
  • Syngas a mixture of hydrogen and carbon monoxide
  • syngas can be used in multiple applications.
  • syngas can be used for producing ammonia or methanol, as a combustible fuel or as a precursor product in the synthesis of liquid fuels via the Fischer-Tropsch processes.
  • Syngas is mainly produced nowadays by steam reforming or partial oxidation of a hydrocarbon fuel gas such as natural gas.
  • Chemical-looping reforming of methane (CLRM) is a promising but less mature pathway for producing syngas that splits the methane reforming process into two reactions by utilizing a nonstoichiometric metal oxide as an oxygen carrier.
  • the two reaction steps are: 1) endothermic reduction of the metal oxide to facilitate the partial oxidation of methane (POM), followed by 2) exothermic re-oxidation of the metal oxide via CO2 and/or H2O splitting to form additional CO and/or H2, respectively.
  • Equations 1 and 2a/2b summarize these reactions for a generic metal oxide (M x O y ) with 5 representing the oxygen nonstoichiometry.
  • Cerium dioxide (CeO2) is known for being capable of use as a nonstoichiometric material used for CLRM due to generally rapid redox kinetics and favorable thermodynamic properties. CeO2 readily re-oxidizes under a wide range of conditions and maintains a stable cubic fluorite structure over a wide range of nonstoichiometry, contributing to high oxygen exchange capacity.
  • the present invention provides for a process for the thermochemical production of a fuel gas in which the loss in yield and selectivity can be countered, and thereby provides a solution that permits the continuous operation of a reactor over many CLRM cycles.
  • the inventors have found that a loss in yield and selectivity can be mitigated essentially by controlling the oxygen nonstoichiometry 5 in the metal oxide in the downstream end, or the downstream end section, of the metal oxide element of the reactor. As a consequence, it was possible to increase the overall selectivity of carbon monoxide Sco from below 0.95 to above 0.95.
  • Fig. 1 shows the evolution of b avg over 30 CLRM cycles at 800°C on a Ni-CeCh reactor when all cycles are kept identical (lozenges) and when cycles are periodically extended according to the invention (circles).
  • the value of b avg is shown oscillating between a reduction half-cycle (higher value of b avg ) and an oxidation half-cycle (lower value of b avg ), and where at each 5 th cycle, the values of b avg are shifter towards higher values of b avg .
  • Fig. 2 shows the evolution of the selectivity of carbon monoxide (Sco) over 30 CLRM cycles at 800°C on a Ni-CeCh reactor when all cycles are kept identical (lozenges) and when cycles are periodically extended according to the invention (circles).
  • Sco carbon monoxide
  • Fig. 2 shows the evolution of the selectivity of carbon monoxide (Sco) over 30 CLRM cycles at 800°C on a Ni-CeCh reactor when all cycles are kept identical (lozenges) and when cycles are periodically extended according to the invention (circles).
  • the selectivity is shown to progressively increase over three cycles following the periodic extension to 0.98, before decreasing again over two cycles towards 0.95, and so on.
  • cycles plateaus around 0.95.
  • the fuel gas that is obtained is preferably a mixture of carbon monoxide and hydrogen, also known as syngas.
  • Syngas may be used as-is as fuel, or may be further used as a feedstock in a process to provide liquid fuels via the Fischer-Tropsch process.
  • the preferred range of ratio between CO/H2 is of from 1 .8 to 2.5.
  • the predetermined duration of the reduction half-cycle may be 60 s or 120 s, and the predetermined duration of the oxidation half-cycle may be 120 s or 150 s.
  • the predetermined duration of the reduction half-cycle is 60 s or 120 s, it may be periodically prolonged to 90 s or 150s, respectively.
  • the predetermined duration of the reduction half-cycle and the predetermined duration of the oxidation halfcycle may be the same or different, and in particular, the duration of the predetermined duration of the reduction half-cycle may be larger than the predetermined duration of the oxidation half-cycle.
  • the predetermined duration of the reduction halfcycle is may be 180 s
  • the predetermined duration of the oxidation half-cycle may be 150 s
  • the predetermined duration of the reduction half-cycle is may be about 20 to 25% larger than predetermined duration of the oxidation half-cycle.
  • the thermochemical reactor comprises a metal oxide element as the catalytically active material that enables the thermochemical production of the fuel gas from feed gas.
  • the metal oxide element may be in different shapes and forms.
  • the metal oxide element may be in the form of a monolithic unit or in the form of a packed bed of individual metal oxide subunits.
  • the metal oxide element may be formed by a plurality of subunits, which may be identical, such as for example a metal oxide element formed of a plurality of identical tubular or ring-shaped subunits.
  • the metal oxide is preferably provided in a form that ensures a high surface-to-volume ratio to increase the contact surface between the metal oxide and the feed gas.
  • the metal oxide is preferably a metal oxide foam such as an opencell metal oxide foam.
  • the metal oxide element is an elongated metal oxide element.
  • the feed gas which is either an oxidant gas or a reductant gas, flows across the elongated metal oxide element along the longitudinal axis of the elongated metal oxide element, by entering the upstream end of the elongated metal oxide element.
  • the feed gas is transformed to carbon monoxide and hydrogen, i.e. syngas, which syngas exits the downstream end of the elongated metal oxide element.
  • a preferred example of an elongated metal oxide element is a tubular packed bed metal oxide element.
  • the metal oxide M x O y -5 of the metal oxide element is in a non- stochiometric redox state.
  • the non-stochiometric redox state is quantified by 5, which denotes a non-zero positive real number and by x, y which denote a natural integer, with the proviso that y is larger than 5.
  • 5 is increased to enhance the selectivity, in particular the selectivity for CO.
  • 5 is increased to a value of at least 0.05, preferably to a value of at least 0.1 and of up to 0.25, and preferably of up to 0.5.
  • 5 is increased to enhance the selectivity, in particular the selectivity of carbon monoxide.
  • 5 is increased to a value of at least 0.05, preferably to a value of at least 0.1 and of up to 0.25, and preferably of up to 0.5.
  • the inventors have found that when the oxygen nonstoichiometry 5 in the metal oxide of the metal oxide element is controlled at the downstream end, or at the downstream end section, of the metal oxide element, a better yield and selectivity may be achieved.
  • the metal oxide is ceria (CeCh-s) or Ni-ceria (Ni-CeCh-s)
  • it is possible to increase the overall selectivity of carbon monoxide Sco by maintaining 5 at a value of at least 0.05, preferably of at least 0.1 and of up to 0.25, and preferably of up to 0.5 at the downstream end, or at the downstream end section, of the metal oxide element.
  • While 5 may not be directly measured, it can be determined by determining the composition of the gas exiting the downstream end, or the downstream end section, of the of the metal oxide element. For example, it is possible to analyse the composition and/or flow rates of the gas exiting the downstream end, or the downstream end section, of the metal oxide element using a mass spectrometer or an infrared spectrometer.
  • hydrogen, carbon dioxide and methane may be determined qualitatively and quantitatively, which allows to calculate the selectivity, for example with respect to carbon monoxide (Sco), which in turn allows calculating 5 of the metal oxide at the downstream end, or the downstream end section, of the of the metal oxide element.
  • cycles of chemical-looping reforming of hydrocarbon (CLRH) are repeated while the reactor is operating.
  • Chemical-looping reforming of hydrocarbon (CLRH) cycle comprises a reduction half-cycle and an oxidation half-cycle, which are induced by feeding the reactor either reductant gas or oxidant gas, respectively, as feed gas, in an alternating fashion.
  • the metal oxide in a non-stochiometric redox state is reduced by contacting a flow of reductant gas comprising a hydrocarbon with the metal oxide M x O y -5ox for a predetermined duration.
  • the hydrocarbon of reductant gas gets oxidized to carbon monoxide, the metal oxide is reduced in its non-stochiometric redox state, and 5 (from 5 0X towards 5 re d) increases.
  • the metal oxide in a non-stochiometric redox state is oxidized by contacting a flow of oxidant gas comprising carbon dioxide, steam and/or a mixture thereof, for a predetermined duration.
  • oxidant gas comprising carbon dioxide, steam and/or a mixture thereof
  • the carbon dioxide and/or steam of the oxidant gas get reduced to carbon monoxide and/or hydrogen
  • the metal oxide is oxidized in its non-stochiometric redox state , and 5 (from 6 re d towards b ox ) decreases.
  • 5 is maintained to be in a range of from 0.05 to 0.5 at the downstream end, or at the downstream end section, of the metal oxide element by periodically increasing the duration of the reduction half-cycle, by increasing the flow rate of flow of reductant gas, or by increasing both the duration of the reductant half-cycle and the flow rate of flow of reductant gas, during a chemical-looping reforming of hydrocarbon (CLRH) cycle.
  • CLRH chemical-looping reforming of hydrocarbon
  • thermochemical reactor When the thermochemical reactor is run repetitively over several identical cycles of chemical-looping reforming of hydrocarbon (CLRH), the selectivity of the thermochemical reactor, and consequently, 5, exhibits a drift towards lesser selectivity, or lesser values of 5.
  • the reduction half-cycle, in which the metal oxide is reduced may be periodically prolonged to re-establish a higher value of 5 at the downstream end section of the metal oxide element, or the flow rate of the reductant gas may be increased to re-establish a higher value of 5 at the downstream end section of the metal oxide element, or both measures may be leveraged simultaneously.
  • thermochemical reactor may be run again for a number of repeating cycles of chemical-looping reforming of hydrocarbon (CLRH), until 5 at the downstream end section falls below a threshold value, i.e. below a value of 0.1 or below a value of 0.05.
  • CLRH chemical-looping reforming of hydrocarbon
  • the metal oxide is a La-Sr-Mn-based perovskite, a ceria (CeCh), and preferably is Ni- ceria.
  • the metal oxide is Ni°-ceria, preferably having a Ni content of from 1 to 10 wt%, more preferably of from 4 to 8 wt%, based on weight of Ni°-ceria.
  • Ni-ceria is obtained by means of a deposition of metallic Ni on the surface of CeC>2 particles via an incipient wetness impregnation method, in particular on the surface of CeC>2 particles having a diameter of about 500 to 1400 pm.
  • the thermochemical reactor is operating below 1000°C, preferably between 650°C and 950°, more preferably between 700°C and 800°. While the thermochemical reactor is capable of operating at temperatures below 650°C, the kinetics of the thermochemical production slow considerably to a point where it becomes impractical for fuel production.
  • the periodicity is every N chemical-looping reforming of hydrocarbon (CLRH) cycles, wherein N being a non-zero integer and preferably is at least 2, preferably is of from 2 to 25, preferably of from 2 to 15. It is understood that the periodicity will depend on parameters such as the feed gas, the metal oxide, but the principle remains in that at some point, after a number of repeating cycles of chemical-looping reforming of hydrocarbon (CLRH), the higher value of 5, of at least 0.05 or at least 0.1 is re-established.
  • CLRH chemical-looping reforming of hydrocarbon
  • the periodicity is every 4 to 10 chemical-looping reforming of hydrocarbon (CLRH) cycles, preferably every 4, 5 or 6 chemical-looping reforming of hydrocarbon (CLRH) cycles. It is understood that the periodicity will depend on parameters such as the feed gas, the metal oxide, but the principle remains in that at some point, after a number of repeating cycles of chemical-looping reforming of hydrocarbon (CLRH), the higher value of 5 will need to be re-established.
  • the need to increase the duration of the flow of the reductant gas, or the mass flow rate of the reductant gas can be determined by measuring the composition of the gas exiting the reactor on the downstream side and in particular by determining the amount of carbon monoxide exiting the reactor on the downstream end of the reactor.
  • the appropriate periodicity and extent of the reduction half-cycle can be determined for a given metal oxide and a given reaction conditions.
  • selectivity of carbon monoxide falls below 0.95
  • adjusting the reduction half-cycle is appropriate, because in that case, 5 will have fallen below a value of 0.1 , or below 0.05.
  • thermochemical reactor comprising a metal oxide element in a non-stochiometric redox state
  • duration of the reduction half-cycle when the duration of the reduction half-cycle is increased, without changing the flow rate of flow of reductant gas, it is increased by at least 25%, preferably 50%, more preferably by 60% and most preferably by up to 100%.
  • thermochemical reactor comprising a metal oxide element in a non-stochiometric redox state
  • the flow rate of the reduction half-cycle when the flow rate of the reduction half-cycle is increased, without changing the duration of flow of reductant gas, it is increased by at least 25%, preferably 50%, more preferably by 60% and most preferably by up to 100%.
  • the reductant gas comprises, or consists of, a hydrocarbon gas chosen from methane, ethane, propane, butane, and mixtures thereof.
  • the reductant gas comprises methane, in combination with ethane, propane, butane, and mixtures thereof, and more preferably comprises at least 50% by weight of methane, and even more preferably comprises at least 75% by weight of methane, in combination with ethane, propane, butane, and mixtures thereof.
  • the reductant gas is methane.
  • the reductant gas comprises less than 5 % by weight, preferably less than 3 % by weight of a non-hydrocarbon gas, in particular of an inert gas.
  • Inert gases may for example be nitrogen, as well as noble gases, such as argon or helium.
  • the oxidant gas comprises, or consists of, carbon dioxide or a mixture of carbon dioxide and steam.
  • the oxidant gas comprises more than 75 % by weight, preferably less than 95 % by weight of a carbon dioxide and/or steam, and in particular is carbon dioxide, steam or a mixture of carbon dioxide and steam. Further the oxidant gas comprises less than 5 % by weight, preferably less than 3 % by weight of an inert gas.
  • Inert gases may for example be nitrogen, noble gases, such as argon or helium. Inert gases may for example be nitrogen, noble gases, such as argon or helium.
  • the duration of the reduction half-cycle is increased, without changing the duration of flow of reductant gas, by at least 15 s. 20 s, 30 s or 60 s.
  • the production of a fuel gas was carried out in a horizontal thermochemical tube reactor made of an alumina tube of 4 mm diameter and comprising a metal oxide element having a weight of 1 gram and made of a Ni-CeO2, where the amount of particles of Ni° deposited on the surface of the ceria was about 5 weight percent.
  • This redox material was synthesized by depositing metallic Ni on the surface of CeO2 particles having a diameter 500 to 1400 pm diameter via an incipient wetness impregnation method
  • Gas flow to the reactor was regulated via three mass flow controllers (MKS GE50A), and the operating temperature was set and maintained using a Carbolite furnace (Carbolite STF 16/180). All gas flow rate and temperature inputs were controlled via a custom LabVIEW program. Downstream gas analysis consisted of a mass spectrometer (HPR-20 QIC, Hiden Analytical) to measure flow rates of H2 and CO2, as well as an infrared (IR) analyzer (Siemens Ultramat 23) to quantify flow rates of CH4 and CO.
  • MKS GE50A mass flow controllers
  • IR infrared
  • the reactor was operated for 30 CLRM cycles at a temperature of 800°C. Total flow rate during each step was set to 100 seem, corresponding to a gas velocity of 0.135 m/s.
  • the reaction time t re d was increased by 50%, i.e. from 60 s to 90 s.
  • the final t ox was set to 15 min for both experiments to ensure complete oxidation of Ni- CeO2.
  • Syngas was produced according to the method of the present invention for the production of a fuel gas in a thermochemical reactor comprising a metal oxide element in a non- stochiometric redox state, and according to a method in which the cycles are kept identical.
  • the two methods are compared over 30 CLRM cycles at 800°C.
  • the method of the present invention for the production of a fuel gas in which the duration of the reduction step is increased periodically reaches a higher selectivity Sco in the ensuing cycles when compared to a method in which the duration of the reduction step is kept constant (in black, lozenges) over the 30 CLRM cycles.
  • the selectivity Sco of the periodic method increases above the selectivity Sco of about 0.95 seen in the constant method after the prolongation of the reduction step during the 10 th , 15 th , 20 th and 25 th CLRM cycle.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Hydrogen, Water And Hydrids (AREA)

Abstract

La présente invention concerne un procédé de production thermochimique d'un gaz combustible tel que du gaz de synthèse dans un réacteur, par l'intermédiaire d'un procédé en boucle chimique qui comprend un procédé de reformage d'un hydrocarbure tel que par exemple du méthane et un procédé de séparation de dioxyde de carbone, ainsi qu'un dispositif pour la production d'un procédé de production thermochimique d'un gaz combustible tel qu'un gaz de synthèse.
PCT/EP2024/067535 2023-06-22 2024-06-21 Reformage en boucle chimique d'hydrocarbures Pending WO2024261301A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US202363522490P 2023-06-22 2023-06-22
US63/522,490 2023-06-22
EP23185886 2023-07-17
EP23185886.1 2023-07-17

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WO2024261301A1 true WO2024261301A1 (fr) 2024-12-26

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180207599A1 (en) * 2015-07-07 2018-07-26 University Of Newcastle Upon Tyne Chemical looping
WO2020058263A1 (fr) * 2018-09-18 2020-03-26 ETH Zürich Procédé de production de gaz de synthèse
US20210113996A1 (en) * 2017-06-05 2021-04-22 North Carolina State University Promoted mixed oxides for "low-temperature" methane partial oxidation in absence of gaseous oxidants

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180207599A1 (en) * 2015-07-07 2018-07-26 University Of Newcastle Upon Tyne Chemical looping
US20210113996A1 (en) * 2017-06-05 2021-04-22 North Carolina State University Promoted mixed oxides for "low-temperature" methane partial oxidation in absence of gaseous oxidants
WO2020058263A1 (fr) * 2018-09-18 2020-03-26 ETH Zürich Procédé de production de gaz de synthèse

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
KANG DOHYUNG ET AL: "Chemical looping partial oxidation of methane with CO2 utilization on the ceria-enhanced mesoporous Fe2O3 oxygen carrier", FUEL, vol. 215, 1 March 2018 (2018-03-01), GB, pages 787 - 798, XP055939914, ISSN: 0016-2361, DOI: 10.1016/j.fuel.2017.11.106 *

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