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WO2025073666A1 - Exploitation de dépôts d'hydrogène naturel par pyrolyse de méthane - Google Patents

Exploitation de dépôts d'hydrogène naturel par pyrolyse de méthane Download PDF

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Publication number
WO2025073666A1
WO2025073666A1 PCT/EP2024/077547 EP2024077547W WO2025073666A1 WO 2025073666 A1 WO2025073666 A1 WO 2025073666A1 EP 2024077547 W EP2024077547 W EP 2024077547W WO 2025073666 A1 WO2025073666 A1 WO 2025073666A1
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Prior art keywords
hydrogen
hydrocarbon
pyrolysis
natural
carbon
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English (en)
Inventor
Gunnar Hennig
Dominique Moulin
Dieter Flick
Daniela Rieck
Jens Peter JOHANNSEN
Thomas Wild
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BASF SE
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BASF SE
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Classifications

    • 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
    • C01B3/22—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
    • C01B3/24—Production of hydrogen or of gaseous mixtures containing a substantial proportion of 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
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/22—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
    • C01B3/24—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons
    • C01B3/28—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons using moving solid particles
    • C01B3/30—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons using moving solid particles using the fluidised bed technique
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH OR ROCK DRILLING; MINING
    • E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
    • 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
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465—Composition of the impurity
    • C01B2203/049—Composition of the impurity the impurity being carbon
    • 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
    • C01B2203/14—Details of the flowsheet
    • C01B2203/148—Details of the flowsheet involving a recycle stream to the feed of the process for making hydrogen or synthesis gas
    • 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
    • C01B2203/16—Controlling the process
    • C01B2203/169—Controlling the feed

Definitions

  • the present invention relates to a process of treatment of raw natural hydrogen-hydrocarbon mixtures that is produced naturally within the Earth's crust, mantle and/or core containing hydrogen in the range of 5 to 95 Vol% and gaseous hydrocarbons, especially methane, in the range of 5 to 95 Vol%, more preferably containing hydrogen in the range of 10 to 80 Vol% and gaseous hydrocarbons, especially methane, in the range of 20 to 90 Vol% in relation to the total volume of the hydrogen-hydrocarbon mixtures, wherein the natural hydrogen-hydrocarbon mixture is fed into a hydrocarbon pyrolysis unit and the hydrocarbons are pyrolyzed into hydrogen and solid carbon and wherein the solid carbon is separated from the hydrogen product stream.
  • methane pyrolysis is considered a promising sustainable technology for future hydrogen production.
  • methane pyrolysis is used to produce highly pure carbon, e.g. carbon nanotube.
  • US 2022/0306462 discloses a method for producing highly pure hydrogen by coupling hydrocarbon pyrolysis with electrochemical hydrogen separation. It is disclosed that the thermal decomposition can be carried out in a fixed-bed reactor, fluidized-bed reactor or moving-bed reactor. Natural gas is typically used as feedstock for the hydrocarbon pyrolysis. It is disclosed that the natural gas is pre-purified by catalytic desulfurization before said pyrolysis. The hy- drogen-depleted anode off-gas of the electrochemical hydrogen separation is recycled and mixed with the natural gas feedstock resulting in a feed mixture of natural gas and up to 20 Vol% hydrogen from the off-gas.
  • WO 2023/059520 describes a hydrocarbon pyrolysis in a plasma reactor.
  • Natural hydrogen also known as “golden”, “white”, “native” or “geologic” hydrogen, is a term used to describe hydrogen that is produced naturally within the Earth's crust, mantle and/or core and is a potential source of most economical and sustainable hydrogen, although the exploration and development had just begun. It is called “golden” or “white” due to its potential benefits as an environmentally friendly fuel, which did not emit any CO2 during its formation.
  • the extraction part will probably be similar to that of natural gas: Most likely a hole supported by a cemented pipe and a stepwise-drilling method to maintain pressure uniformity will be used as described in [3], Likewise secondary and enhanced recovery methods will be applied to maximize deposit yields.
  • the first steps of gas-treatment will be similar to those used in natural gas extraction:
  • solid particles e.g. sands
  • liquids e.g. water, oil
  • gases e.g. hydrocarbons, hydrogen
  • the subsequent treatment methods to receive the hydrogen in pure form will then differ from natural gas processing:
  • mixtures of hydrogen and methane could be used for the energetic use , e.g. for heat or power generation by combustion, it can be assumed that political and regulatory pressure will continue to increase and that such possibilities will be heavily regulated in the coming years due to the associated CO2 emissions.
  • PSA pressure swing adsorption
  • cryogenic distillation amine-based absorption
  • amine-based absorption amine-based absorption
  • Another disadvantage of the mentioned technologies to purify hydrogen could be a changing gas composition during exploitation. As described for a deposit in north-east France, H2 concentrations in natural hydrogen could change as a function of depth by a factor of 10. A dedicated hydrogen purification plant is designed for a specific load case. If boundary conditions (such as input concentrations) change beyond this range, additional equipment would be necessary or existing ones must be modified, which would involve further costs.
  • This task is solved by the present invention relating to a process of treatment, especially a process of combined purification and hydrogen production, of raw natural hydrogen-hydrocarbon mixtures containing hydrogen that is produced naturally within the Earth's crust, mantle and/or core in the range of 5 to 95 Vol% and gaseous hydrocarbons (especially methane) in the range of 5 to 95 Vol%, more preferably containing hydrogen in the range of 10 to 80 Vol% and gaseous hydrocarbons (especially methane) in the range of 20 to 90 Vol%, wherein the natural, hydrogenhydrocarbon mixture is fed into a hydrocarbon pyrolysis unit and the gaseous hydrocarbons, especially methane, are pyrolyzed into hydrogen and solid carbon and wherein the solid carbon is separated from the hydrogen product stream.
  • a process of treatment especially a process of combined purification and hydrogen production
  • gaseous hydrocarbons By pyrolyzing the gaseous hydrocarbons into hydrogen and solid carbon sulfur-containing components can be tolerated and can be separated conventionally downstream of the hydrocarbon pyrolysis unit.
  • other gas components such as N2, CO2, He, Ar, do not interfere with the reaction and can also be separated conventionally downstream of the hydrocarbon pyrolysis unit.
  • the extracted and pre-processed natural hydrocarbon-hydrogen mixtures typically contain from 5 to 95 Vol%, preferably 5 to 90 Vol%, more preferably 25 to 90 Vol%, even more preferably 50 to 90 Vol%, even more preferably 75 to 90 Vol%, hydrogen, and 5 to 95 Vol%, preferably 10 to 95 Vol%, more preferably 10 to 75 Vol%, even more preferably 10 to 50 Vol%, even more preferably 10 to 25 Vol%, methane and higher hydrocarbons (C2-C6), and additional components, such as N2, H2S, CO2, Helium, Argon, etc.
  • the composition of the raw natural hydrogen-hydrocarbon mixtures might fluctuate depending on the drilling depth.
  • the hydrogen and hydrocarbon contain might therefore fluctuate in the range of +/- 5 to 50 Vol.-%, preferably +/- 5 to 30 Vol.-%.
  • the composition of the naturally produced hydrogen-hydrocarbon mixture drilled, pretreated and fed into the reactor preferably varies and/or fluctuates between a molar ratio of hydrogen to hydrocarbon from 20 to 0.05, preferably from 15 to 1, even more preferably from 10 to 3, during the pyrolysis process.
  • the ratio of hydrogen to hydrocarbon of the naturally produced hydrogen-hydrocarbon mixture fed into the pyrolysis reactor is therefore not constant during the process.
  • methane pyrolysis In hydrocarbon pyrolysis, mainly named methane pyrolysis (reaction equation (1)), hydrogen is obtained from methane, which is usually to come from natural gas, synthetic methane, industrial off gas, e.g. cracker off gas, biogas or sewage gas.
  • methane which is usually to come from natural gas, synthetic methane, industrial off gas, e.g. cracker off gas, biogas or sewage gas.
  • methane pyrolysis is considered a promising sustainable technology for future hydrogen production.
  • the generic term methane pyrolysis covers a wide range of different process technologies. The best known and most advanced of these are:
  • the solid carbon type generated in the methane decomposition depends on the reaction conditions, reactor and heating technology. Examples are carbon black from plasma processes carbon powder from liquid metal processes granular carbon from thermal decomposition in fixed, moving or fluidized bed reactors.
  • a plasma with >3000 °C is generated in which the natural gas, is pyrolyzed.
  • the gas mixture leaves the reactor at temperatures between 900 - 2000 °C.
  • Catalysts can also be used to reduce the high reaction temperatures (see for example WC2011029144, WC2016154666).
  • hydrocarbon preferably methane
  • pyrolysis a very cost-effective alternative is the use of iron oxide catalysts. Reaction temperatures of approx. 700 to 1000°C can be realized.
  • the reactions take place, for example, in the fluidized bed, with the catalyst as the fluidized material.
  • the methane is decomposed at the catalytic surface.
  • Another advantage is that the carbon can be deposited on the particles. This reduces the density of the particles and, after sufficient deposition of carbon, they can be discharged from the reactor with the gas flow. This could be controlled by gas flow and the pressure of the fluidized bed reactor.
  • the hydrocarbon, in particular methane, decomposition is preferably conducted in a moving, fluidized 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.
  • methane decomposition is also referred to as methane pyrolysis since no oxygen is involved.
  • the decomposition can be conducted in different ways known to the persons skilled in the art: catalytically or thermally, and with heat input via plasma, microwave, heated carrier gas, resistance heating, induction, liquid metal processes or autothermal.
  • 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 decomposition process is located at an existing chemical production site.
  • 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 containing the raw natural, golden hydrogen-hydrocarbon mixture and optionally additional hydrogen if needed. Due to the fact that the total feed concentration of the reactor could be controlled by the internal hydrogen recycle there is a broad range for the concentration of hydrogen in the natural hydrogen-hydrocarbon mixture applicable.
  • the hydrogen and/or hydrocarbon concentration of the raw natural, golden hydrogen-hydrocarbon mixture is measured before feeding it into the pyrolysis unit.
  • the direct hydrogen product stream recycle is increased or decreased during the pyrolysis process (see Figures 4 and 5).
  • additional hydrogen is added to the pyrolysis unit for adjusting, preferably continuously adjusting, the concentration to the operation point.
  • additional hydrocarbons like natural gas or biomethane, are added to the pyrolysis unit for continuously adjusting the concentration to the operation point.
  • the substrate can either be a support substrate in the reactor (a pre-installed part) or a granular material.
  • the preferred substrate is a carbon-containing substrate, for example pyrolytic carbon itself.
  • the particle size of a preferred substrate is in the range of 0.1 to 10 mm, preferably 0.3 to 8 mm, even more preferably 1 to 8 mm, even more preferably 2 to 8 mm.
  • 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 wt.-% to 100 wt.-%, preferably 99 wt.-% to 100 wt.-%, even more preferably 99.5 wt.-% to 100 wt.-% and a content of alkaline-earth metals, transition metals and metalloids of 0 and 2 wt.-%, preferably 0 to 1 wt.-%, even more preferably 0 to 0.5 wt.-%, 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-%.
  • 90 weight-% of the carbon of the granular pyrolytic carbon composition is not-functionalized, preferably 95 weight-%, even more preferably 98 weight-%, especially 99 weight-%, wherein carbon functionalization refers to a reaction in which a carbon-carbon bond is broken and replaced by a carbon-X bond (where X is usually hydrogen, oxygen, sulfur, phosphorus, nitrogen, halogens, and/or metals).
  • the cation exchange capacity (CEC) of granular pyrolytic carbon is about 0.01 to 1.5 cmol/kg, preferably 0.025 to 0.75 cmol/kg.
  • the porosity of the granular pyrolytic carbon is between 0% to 15%, preferably 0.2% to 10%, most preferably 0.2% to 5% (Hg porosimetry, DIN66133).
  • 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 hydrogen and granular pyrolytic carbon are produced from hydrocarbons present in the raw natural hydrogen-hydrocarbon mixtures, preferably methane comprises: a reactor surrounding a reactor interior the reactor is configured to provide a gravity-driven moving bed in a reaction zone of the reactor interior, which gravity-driven moving bed comprises a large number plurality of solid substrates, wherein the reactor is also configured to guide natural produced hydrogen-hydrocarbon mixture into the reaction zone, wherein, in order to heat natural produced hydrogen-hydrocarbon mixture, the reactor is configured to heat the solid substrates in the reaction zone by generating an electric current in the solid substrates between a pair of first and second electrodes such that, by transferring heat from the solid substrates to natural produced hydrogen-hydrocarbon mixture, natural produced hydrogen-hydrocarbon mixture in the reaction zone can be heated to a reaction temperature to produce hydrogen and granular pyrolytic carbon, and wherein the reactor interior also comprises a first heat integration zone in which heat from hydrogen produced in the
  • - withdrawn hydrogen is preferably at least partly recycled and introduced into the reactor.
  • a fixed bed technology is used for the hydrocarbon pyrolysis of the present invention comprising:
  • the solid substrates are heated in the reaction zone, preferably the solids are electrically heated, more preferably the solids are heated via a direct electric Joule heating, - natural produced hydrogen-hydrocarbon mixture is introduced into the reaction zone, wherein the natural produced hydrogen-hydrocarbon mixture is contacted with the heated solid substrates in the reaction zone, wherein heat from the heated solid substrates is transferred to natural produced hydrogen-hydrocarbon mixture in order to heat natural produced hydrogen-hydrocarbon mixture in the reaction zone and wherein natural produced hydrogen-hydrocarbon mixture is decomposed to hydrogen and pyrolytic carbon that is deposited on the solid substrates in the reaction zone, preferably natural produced hydrogen-hydrocarbon mixture is introduced via the top of the reactor,
  • cyclic mode operation e.g. One reactor is in production mode and carbon is deposed in the fixed bed until the maximum carbon deposition is reached. While the carbon is removed from this reactor, the next reactor starts with production and so on. With this cyclic operation mode, a continuous production is ensured.
  • a fluidized bed technology is used for the hydrocarbon pyrolysis of the present invention comprising:
  • a plurality of solid substrates having a particle size of 0.1 to 10 mm is introduced in the fluidization zone, the reaction zone, and placed on a distributor o optionally the substrates are heated externally and are introduced into the reactor at a temperature of 800 °C to 1500 °C
  • - natural produced hydrogen-hydrocarbon mixture is introduced into the reactor via the bottom, distributed by the distributor fluidizing the solid substrates and guided through the reaction zone wherein natural produced hydrogen-hydrocarbon mixture is contacted with the heated solid substrates in the reaction zone, wherein heat from the heated solid substrates is transferred to natural produced hydrogen-hydrocarbon mixture in order to heat natural produced hydrogen-hydrocarbon mixture in the reaction zone, wherein natural produced hydrogen-hydrocarbon mixture is decomposed to hydrogen and pyrolytic carbon that is deposited on the solid substrates in the reaction zone, o Due to the relative motion of the particles in a fluidized, bed relative carbon depositions from the pyrolyzed gas on the solid granule per pass through the reactor are preferred above 10 w% and more preferred above 20 w%. The relative deposition is related to the mean solid particle mass flux out of the reactor. o The pressure is preferably 1 to 10 bar.
  • - withdrawn substrate is preferably at least partly recycled and introduced into the reactor
  • - withdrawn hydrogen is preferably at least partly recycled and introduced into the reactor.
  • Fluidized bed reactors are known in the state of the art, e.g. Werther, Ullmanns's encyclopedia of industrial chemistry Fluidized Bed-Reactors, 2012 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.
  • a fluidized bed reactor may have more than one stage as described in W02022081170 and US20210331918.
  • the raw hydrogen product stream is purified in one or more removal apparatus, e.g. using adsorption or membrane technologies.
  • the hydrogen product stream can still contain hydrogen sulfide.
  • Hydrogen sulfide can preferably be removed from the gaseous product stream via gas scrubbing, e.g. via ZnO, CuZnO, Fe(OH)3, Zeolites, MOFs, as known in the state of the art.
  • the hydrogen product stream can still contain carbon oxide, hydrocarbons and 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.
  • methane pyrolysis can also be used for combined purification and hydrogen production, thus circumventing the disadvantages of natural hydrogen extraction and further treatment steps described above.
  • a high-purity carbon that can be used sustainably should significantly increase the chances of realizing a methane pyrolysis process, not only from an economic point of view.
  • Fig 1 shows the block diagram of a general embodiment of the process of the invention.
  • the inventive examples show that the use of methane pyrolysis for combined purification and hydrogen production converts the hydrocarbons in the natural, golden hydrogen feed into additional hydrogen and valuable carbon in one step, generates low CO2 emissions and is flexibly useable even with fluctuating hydrogen concentrations in the feed. Furthermore, the hydrogen (both natural and resulting from the hydrocarbon) is obtained as a product stream with a high purity, independently of the fluctuating hydrogen concentrations in the feed. Thus, the inventive examples show both the purification of natural hydrogen and the production and purification of additional (turquoise) hydrogen.

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Abstract

La présente invention concerne un procédé de traitement de mélanges hydrocarbures-hydrogène doré naturel brut contenant de l'hydrogène produit naturellement dans la croûte, le manteau et/ou le noyau de la Terre dans la plage de 5 à 95% Vol et des hydrocarbures gazeux, notamment du méthane, dans la plage de 5 à 95% Vol, plus préférentiellement contenant de l'hydrogène dans la plage de 10 à 80% Vol et des hydrocarbures gazeux, notamment du méthane, dans la plage de 20 à 90% Vol par rapport au volume total des mélanges hydrocarbures-hydrogène, le mélange hydrocarbures-hydrogène doré naturel étant introduit dans une unité de pyrolyse d'hydrocarbures et les hydrocarbures étant pyrolysés en hydrogène et carbone solide et le carbone solide étant séparé du flux de produit d'hydrogène.
PCT/EP2024/077547 2023-10-06 2024-10-01 Exploitation de dépôts d'hydrogène naturel par pyrolyse de méthane Pending WO2025073666A1 (fr)

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US2982622A (en) 1958-09-02 1961-05-02 Exxon Research Engineering Co Hydrocarbon conversion process
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US20040141654A1 (en) 2003-01-17 2004-07-22 Yi-Yung Jeng Texture encoding procedure
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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