EP3638620A1 - Procédé et système pour éviter et/ou réduire la quantité de suie - Google Patents

Procédé et système pour éviter et/ou réduire la quantité de suie

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Publication number
EP3638620A1
EP3638620A1 EP18730971.1A EP18730971A EP3638620A1 EP 3638620 A1 EP3638620 A1 EP 3638620A1 EP 18730971 A EP18730971 A EP 18730971A EP 3638620 A1 EP3638620 A1 EP 3638620A1
Authority
EP
European Patent Office
Prior art keywords
gas
soot
electrolysis
hydrogen
synthesis gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP18730971.1A
Other languages
German (de)
English (en)
Inventor
Dietmar Rüger
Carl Berninghausen
Christian Klahn
Sebastian Becker
Robert Blumentritt
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SunFire GmbH
Original Assignee
SunFire GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SunFire GmbH filed Critical SunFire GmbH
Publication of EP3638620A1 publication Critical patent/EP3638620A1/fr
Pending legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
    • B01J19/0026—Avoiding carbon deposits
    • 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
    • C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
    • C01B3/12—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents by reaction of water vapour with carbon monoxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/02—Process control or regulation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00132—Controlling the temperature using electric heating or cooling elements
    • B01J2219/00135—Electric resistance heaters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00245—Avoiding undesirable reactions or side-effects
    • B01J2219/00247—Fouling of the reactor or the process equipment
    • 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
    • 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
    • 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
    • C01B2203/0888—Methods of cooling by evaporation of a fluid
    • 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
    • C01B2203/0888—Methods of cooling by evaporation of a fluid
    • C01B2203/0894—Generation of steam
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry

Definitions

  • the invention relates to a Rußvermeidungs- and / or Rußverminderungs vide for
  • Soot avoidance and / or soot reduction arrangement Soot avoidance and / or soot reduction arrangement.
  • soot solid carbon
  • the formed soot settles on the heat exchanger surface and there leads to a deterioration of the heat transfer and to a blockage of the flow channels.
  • Dirty heat exchanger surfaces reduce the proportion of heat that can be recovered and used from gas cooling. Clogged flow channels increase the
  • the heat exchanger's construction material (carbide formation) can do that to one
  • heat exchanger includes here also pipelines in which the CO-containing gas cools due to insufficient thermal insulation, which also can form soot.
  • heat exchangers in the sense of this disclosure can also be recuperators and the like.
  • the technical field is the cooling of hot, CO-containing gases after their
  • the invention is concerned with how the formation of soot during gas cooling can be suppressed or prevented and how yet formed soot can be removed again from the heat exchanger surface.
  • FIG. 9 shows the state point of a synthesis gas, in order to illustrate the thermodynamic soot formation conditions.
  • the composition of a (synthesis) gas whose individual gases consist only of the components C, O 2 and H 2 , in the C-0 2 -H 2 -Standsdiagramm as a point (point 1) with the coordinates C, 0 2 and H 2 are shown.
  • Gas mixture has reached the limit of absorption capacity of carbon can be represented as an isotherm (soot limit at the corresponding temperature).
  • soot is temperature and pressure dependent as shown in Figures 10 and 11.
  • Fig. 10 shows the synthesis gas composition of an RWGS process as a function of equilibrium temperature at a pressure of 1 bar for a H 2 -CO molar ratio of 2
  • Fig. 11 shows the synthesis gas composition of an RWGS process as a function of equilibrium temperature at a pressure of 10 bar also for a H 2 -CO molar ratio of 2.
  • soot formation during the electrolysis of carbon dioxide in a solid oxide electro-lysing cell can lead to deposits on the electrolysis cells and clogging of the membranes, ultimately stopping the operation of the electrolysis.
  • the synthesis gas 1 in Fig. 9 should have been generated at 950 ° C and 1 bar.
  • the soot limit of 950 ° C lies to the left of point 1. This means that the gas is outside the soot area under these conditions.
  • Reactor outlet temperature is controlled procedurally.
  • the soot limit in the C-0 2 -H 2 diagram applicable for each cooling (inter-) temperature shifts to the right. At about 570 ° C point 1 enters the soot area, assuming the thermodynamic equilibrium state, and remains in this area during further cooling.
  • Fig. 12 shows the course of the carbon activities of reactions R1, R2 and R3 starting from gas 1 (analogous to point 1 at 950 ° C). It is purely thermodynamic to assume soot formation in carbon activities of the single reactions of ac £ 1, with the driving force increasing to higher values a c . At a c ⁇ 1, the reverse reaction is thermodynamically favored.
  • reaction R3 A qualitative statement on the basis of the carbon activities, from which temperature carbon black is formed during the gas cooling, is only possible under the assumption that eg reaction R3 is kinetically strongly inhibited.
  • a first soot formation is ideally carried out only from about 680 ° C by reaction R1, wherein resulting carbon black can be consumed by reaction R2 until it forms thermodynamically soot at temperatures less than 630 ° C.
  • This approach differs from the C-02 H 2 diagram (soot formation ⁇ 570 ° C), in which, as in a chemical reactor, all reactants are in thermodynamic equilibrium at all temperatures, but also has the disadvantage that the complex reaction system and the mutual influence of the reactions is disregarded.
  • Heat exchanger accumulates on the heat exchanger surface and in the flow channels and leads to problems there. Below 350-400 ° C is known to hardly form carbon black at the usual residence times.
  • Natural gas as e.g. is also offered by Uhde and Linde
  • the cooling of the synthesis gas is generally carried out by quenching with WasserAdampf or cooled and recirculated synthesis gas.
  • the problem of soot formation during the Cooling of the synthesis gas is just not described in the prior art of the production of CO-containing gases by gasification and reforming.
  • the applicant's EP 20 49 232 B1 describes a method with the aim of recycling the combustion products carbon dioxide and water, as they occur in the exhaust gases from combustion processes or in the environment, into renewable synthetic fuels and fuels by electrical energy , which was not generated with the help of fossil fuels, but renewable.
  • the technical problem is solved by separating the chemically bound in the combustion process of carbon and hydrogen oxygen from the products of combustion carbon dioxide and water with the introduction of electrical energy, which was primarily using renewable energy sources, but not with the help of fossil fuels produced by according to the invention by electrolysis of water, or preferably steam,
  • the recuperative preheating of the carbon dioxide-hydrogen mixture and its further heating takes place by supplying electrical energy in the presence of catalysts.
  • the water used in the gas and product cooling is to be used together with external water for the direct cooling of the synthesis crude gas and the synthesis processes to vaporize it and to split the steam into electrolysis into hydrogen and oxygen.
  • Condition point 2 only at a temperature ⁇ 300 ° C in the soot area. Due to the very slow kinetics of the soot formation reactions (R1, R2 and R3) at this temperature level, no soot would be likely to form.
  • the water vapor participates in the gas conversion reactions in the RWGS process and alters the gas composition, which also leads to a change in the H 2 -CO molar ratio.
  • the amount of H 2 feed gas must be reduced.
  • the resulting gas composition shows point 3, which reaches the soot area at about 300 ° C.
  • the price of water vapor mixing during gas production is a higher C0 2 content in the product gas.
  • the document WO 2011 133 264 A1 discloses a method / arrangement for the electrochemical reduction of carbon dioxide to the product carbon monoxide at the cathode and supply of a reducing agent to rinse the anode.
  • a reducing agent eg hydrocarbons
  • On the anode side is achieved by the oxidation of the reducing agent (eg hydrocarbons) an efficiency-increasing reduction of the oxygen partial pressure and the heating of the apparatus.
  • the feed streams are heated recuperatively against the product streams.
  • the invention further comprises the additional supply of steam to produce a synthesis gas.
  • the publication WO 2013 131 778 A2 discloses a method / arrangement for producing high-purity carbon monoxide (> 90% by volume) by electrolysis of carbon dioxide, consisting of SOEC stack ( ⁇ 80% conversion) and a special gas separation unit.
  • Other features here are the recirculation of (C0 2 / CO), the C0 2 purging of anode and / or stack housing, cleaning Feed-C0 2 and the pressure increase upstream of the gas separation unit.
  • carbon deposits on the tube wall of the nickel-based material can form behind the stack during the cooling of the CO 2 / CO mixture, which can lead to damage of the material by metal dusting.
  • Document WO 2014 154 253 A1 goes deeper into the recuperative preheating of the feed gases compared to the above-mentioned method / arrangement and proposes further measures for avoiding the formation of carbon deposits and metal dusting in the system, namely quenching with inert gas (C0 2 or N 2 ) to 400-600 ° C to avoid metaldusting, then recuperation for efficiency and further H 2 S admixture in feed and / or downstream, to avoid soot formation in the system (50 ppb ... 2 ppm).
  • inert gas C0 2 or N 2
  • Fig. 14 which illustrates the state points of synthesis gases from co-electrolysis at different H 2 O / C0 2 conversions
  • point 1 shows the feed gas mixture C0 2 and water vapor
  • point 2 the product gas compositions for 80% conversion.
  • State point 3 reached. This point reaches the soot area at a temperature of 550 ° C during gas cooling.
  • a reduction in sales also results in an increase in the C0 2 content in the product gas and thus gas deterioration.
  • oxygen-containing gas in a multi-stage cascade comprising at least one of catalytic autothermal reforming and / or catalytic partial oxidation, wherein each stage of the cascade is supplied with oxygen-containing gas and hydrocarbon feed gas respectively converted to hydrogen-containing process gas and in series all subsequent Cascade goes through.
  • it is a two-stage series circuit comprising in the first stage an allothermal steam methane reformer, and in the second stage a catalytic autothermal reformer, wherein the second stage, the hydrogen-containing process gas of the first stage is fed and additionally hydrocarbon feed gas, steam and oxygen-containing gas is fed, wherein the catalytic autothermal reformer is fed at most 1, 5 times the amount of O 2 , which corresponds to the amount of H 2 , which is formed in the allothermal steam methane reformer, and the hydrocarbon-containing feed gas and the oxygen-containing gas separated be fed from each other via devices that protrude at different levels with different orientation in the last catalytic autothermal reforming stage, wherein the
  • oxygen-containing gas is introduced via at least one separate feed secantially to the center of the circular reactor above the catalyst bed, and the
  • hydrocarbon-containing feed gas is preferably fed axially at the top of the reactor.
  • Water vapor is a necessary reaction partner of methane for the formation of CO and H 2 in this process.
  • additional hydrogen can be generated from the CO formed:
  • the heat required for the reformation reaction can be supplied externally (allothermic) or by partial oxidation of CH 4 and / or H 2 and / or CO with an oxygen-containing oxidant in the process itself (autothermic).
  • introduced water vapor streams 3b, 3c, 3d are correct to the respectively before the other reforming stages 1 b, 1 c and 1 d necessary amount of steam to continue the running in these stages reforming reactions.
  • No additional amount of water vapor is introduced at the end of all process stages in order to suppress or avoid soot formation during gas cooling.
  • the amounts of hydrogen 6a, 6b and 6c introduced into the process stages 1b, 1c and 1c are the amount of hydrogen produced in the preceding process stages and not an additional amount of hydrogen introduced before or at the end of the overall process, which is the formation of soot upon cooling to suppress or prevent the generated gas.
  • WO 2010/020358 A2 is the soot in the production of synthesis gas from hydrocarbon-containing gases by multi-stage allothermic or autothermal steam reforming, in which the supplied water vapor necessary reaction gas and the subsequent process stages supplied hydrogen is produced product and no additional Water vapor or hydrogen for soot prevention and soot suppression is supplied. Since it continues to be the gas generation and not the gas cooling process, the disclosure according to the document
  • WO 2010/020358 A2 with respect to the present invention does not oppose.
  • an electrolysis method with an electrolytic cell using at least one recirculating flushing medium is known.
  • this document relates to an electrolysis device.
  • water vapor and / or carbon dioxide are decomposed electrolytically into hydrogen, carbon monoxide and oxygen.
  • the product gas H 2 / CO is removed from the cathode compartment by means of purge gas (50) and separated into product gas H 2 / CO, purge gas (50) or purge gas-product gas mixture (50 + H 2 / CO) in the gas separation device located behind the electrolysis ,
  • Product gases H 2 / CO are recycled, added to the reactant gas stream before the electrolysis and again as a cathode purge gas for the removal of the electrolysis products H 2 / CO the
  • the purge gas (50) is inert to the
  • the rinsing of the cathode side can also be done by the unreacted portion of the supplied reactant gas (C0 2 / H 2 0), which can also be recycled after gas separation.
  • the document WO 2015/185039 A1 is thus concerned with the provision and the effective use of cathode and anode scavenging gas by the use of a gas separation device downstream of the electrolysis and recycling and reintroduction of the separated purge gas stream as purge gas in the electrolysis.
  • the purge gas does not necessarily have to be H 2 or H 2 O on the cathode side. It must be only inert to CO and H 2 on the cathode side.
  • the document WO 2015/185039 A1 does not therefore relate to soot avoidance or
  • the publication DE 42 35 125 A1 proposes a process for the production of synthesis gas and an apparatus for carrying out this process.
  • synthesis gas fossil materials, such as. As coal or natural gas, as starting materials. This contributes to a further shortage of raw material reserves as well as to an increase in C0 2 emissions.
  • the process of the invention is
  • the carbon dioxide is in particular from the atmosphere or from non-fossil emissions such. B.
  • the publication WO 2014/097142 A1 describes a process for the parallel production of hydrogen, carbon monoxide and a carbon-containing product which is characterized in that one or more hydrocarbons are thermally decomposed and at least part of the resulting pyrolysis gas from the reaction zone of the
  • Carbon dioxide is converted to a carbon monoxide and hydrogen-containing gas mixture, a synthesis gas.
  • the hydrogen is not additionally mixed in the generated synthesis gas in order to avoid the formation of soot in the gas cooling, but serves to set the desired H 2 : CO molar ratio in the finished synthesis gas.
  • the addition of hydrogen-containing gas mixture from the pyrolysis directly into the gas stream after the RWGS process reduces the generatable in the RWGS-level amount of CO, since heat and H 2 is missing for the chemical conversion of C0 2, corresponding to
  • the formed soot settles on the heat exchanger surface and there leads to a deterioration of the heat transfer and to a blockage of the flow channels.
  • Especially the danger of blockage of the flow channels of the gas cooling sections is in large-scale systems such as gasification and reformer systems also because of there usually
  • Quenching is usually of little relevance, but increases as the system size declines (decentralized RWGS or C0 2 / Co electrolyzers).
  • Dirty heat exchanger surfaces reduce the proportion of heat that can be recovered and used from gas cooling.
  • the coating of the catalytically effective heat transfer surface e.g. with Ni / Sn, Cu, suppresses the catalyzed soot formation and is thus able to extend the operating time between two cleaning cycles.
  • the layer protects the construction material from metal dusting.
  • a protective layer can not completely prevent soot formation.
  • Synthesis gas stream achieved with water Possibly formed soot is usually discharged without problems with the excess quench water from the quencher and can be separated by filters from the water.
  • Inert gas quenching such as C0 2 or N 2 , degrades gas quality and would require expensive gas purification processes.
  • Heat exchanger given so that the flow rate increases and the adhering soot can be blown out. Due to the increased flow velocity, the pressure loss via the heat exchanger increases in part considerably. Especially in co-electrolysis with electrolysis cells based on SOC lead strong Pressure fluctuations to impermissibly high differential pressures across the electrolysis cells, which leads to the breakage and thus the destruction of the cells.
  • Knockers for Rußabbgraphy during operation of the system are problematic in that the heat exchangers are used at high gas temperatures 850 ... 950 ° C and a mechanical vibration stress in this temperature range leads to problems in the strength of the materials.
  • soot avoidance and / or Rußverminderungs vide for avoiding and / or reducing soot within a synthesis gas and / or CO-containing gas generating device from the feed gases carbon dioxide, water vapor, hydrogen and / or a hydrocarbon-containing residual gas and electric energy in RWGS processes, electrolysis for the electrochemical decomposition of carbon dioxide and / or water vapor, reforming processes and / or synthesis gas production processes with at least one gas generating unit, an electrolysis stack and / or a heater-reactor combination for carrying out a RWGS reaction, and at least one cooling line / recuperator for CO-containing Gas and / or synthesis gas,
  • an additional gas, liquid and / or gas mixture is added before being fed into the gas production in the feed gas stream and / or after gas production in the CO-containing gas / synthesis gas, wherein the additional gas, liquid and / or gas mixture is selected from:
  • Gas stream is mixed, wherein the hydrogen-rich gas when produced via the separate electrolysis process prior to interference recuperative against
  • soot avoidance and / or soot reduction method for preventing and / or reducing soot within a synthesis gas and / or CO containing gas producing apparatus from the feed gases is carbon dioxide, water vapor, hydrogen and / or a hydrocarbonaceous residual gas and electric power in RWGS processes , Electrolysis for electrochemical decomposition of carbon dioxide and / or water vapor, reforming processes and / or synthesis gas production processes with at least one gas generating unit, an electrolysis stack and / or a heater-reactor combination for performing a RWGS reaction, and at least one CO cooling / Rekuperator -containing gas and / or synthesis gas,
  • soot avoidance and / or soot reduction method for preventing and / or reducing soot within a synthesis gas and / or CO-containing gas producing apparatus from the feed gases is carbon dioxide, water vapor, hydrogen and / or a hydrocarbonaceous residual gas and electric power in RWGS processes , Electrolysis for electrochemical decomposition of carbon dioxide and / or water vapor, reforming processes and / or synthesis gas production processes with at least one gas generating unit, an electrolysis stack and / or a heater-reactor combination for performing a RWGS reaction, and at least one CO cooling / Rekuperator -containing gas and / or synthesis gas,
  • soot-avoidance and / or soot-reduction method is for
  • Cooling section / recuperator for CO-containing gas and / or synthesis gas Cooling section / recuperator for CO-containing gas and / or synthesis gas
  • hydrogen-rich gas for cooling the CO-rich gas stream, this hydrogen-rich gas being externally supplied or produced by separate C0 2 and H 2 0 electrolysis, and the hydrogen rich gas is mixed into the CO-rich gas stream, wherein the hydrogen-rich gas is recuperatively cooled against heated water vapor and / or C0 2 stream when prepared via the separate electrolysis process prior to mixing.
  • soot avoidance and / or Rußverminderungs vide for avoiding and / or reducing soot within a synthesis gas and / or CO-containing gas generating device from the feed gases carbon dioxide, water vapor, hydrogen and / or a hydrocarbon-containing residual gas and electric energy in RWGS- Processes, electrolysis for the electrochemical decomposition of carbon dioxide and / or water vapor, reforming processes and / or synthesis gas production processes with at least one gas generating unit, an electrolysis stack and / or a heater-reactor combination for performing a RWGS reaction, and at least one cooling line / recuperator for CO-containing gas and / or synthesis gas,
  • the soot-avoidance and / or soot-reducing arrangement in particular in conjunction with a soot-evisceration and / or soot-reduction method disclosed herein, on or within a synthesis gas and / or CO-containing gas generating device from the feed gases carbon dioxide, water vapor, hydrogen and / or a hydrocarbon-containing residual gas and electric energy in RWGS processes, electrolyses for the electrochemical decomposition of carbon dioxide and / or water vapor, reforming processes and / or synthesis gas production processes with at least one gas generation unit, an electrolysis stack and / or a heater-reactor combination for carrying out an RWGS reaction , and at least one cooling line / recuperator for CO-containing gas and / or synthesis gas,
  • Gas mixture supply is provided, whereby by this supply water vapor,
  • Hydrogen-rich gas from an external feed device hydrogen-rich gas from a separate C0 2 - and H 2 0 electrolysis and / or water are supplied.
  • Soot reduction and / or soot reduction by increasing the water vapor content in the generated gas :
  • Electric energy consisting of at least one gas generating unit, e.g. a co-electrolysis stack or a heater-reactor combination for carrying out the RWGS reaction, and a recuperative syngas cooling, it is proposed to suppress the soot formation during the gas cooling or possibly avoid, is proposed by admixing water vapor into the synthesis gas after gas production the
  • the Wasserzampfmischung can be done in two ways.
  • the first possibility is that the colder steam (about 150 ° C) is added directly to the approximately 600 ° C hot gas. That would be like a quench with gas. In this case, the product gas loses exergy, and in a recuperative preheating of the feed gases would their
  • the water vapor admixture to the product gas 1 produced may also be at 950 ° C, i. without prior intermediate cooling, immediately before the subsequent gas cooling.
  • any still occurring homogeneous gas reactions can be considered in the adjustment of the product gas composition, for example by varying the amounts of feed gas.
  • the water vapor has in the admixture after the actual gas generation only the task to reduce the formation of soot and suppress at best.
  • the energy content of the steam is not used. It is usually removed to the atmosphere in the final cooling of the gas. Soot reduction and / or soot reduction by H 2 excess
  • Membrane separation plant removed so that the synthesis gas has the desired H 2 -CO molar ratio.
  • the separated hydrogen is recycled by means of a compressor and mixed again with the feed gas stream or the synthesis gas stream.
  • the admixture of hydrogen to the feed gases of a RWGS process or a co-electrolysis shifts the gas toward the hydrogen corner and thus out of the soot area.
  • FIG. 15 the representation of the state points of a co-electrolysis process with H 2 - excess is shown.
  • the state diagram Fig. 15 shows the admixture of a H 2 -rich recycle gas (point 2) to a H 2 0-C0 2 feed gas stream (point 1) before co-electrolysis.
  • the electrolytic decomposition of the mixed gas (point 3) gives the gas after co-electrolysis (point 4).
  • the approximately 850 ° C hot gas at point 4 after co-electrolysis is cooled. Although it enters the soot area at a temperature ⁇ 300 ° C, it will not form soot during cooling due to the low kinetics of soot formation reactions at temperatures below 300 ° C.
  • a disadvantage of quenching with water is that the heat for the product gas cooling is not available, but must be dissipated as condensation heat at low temperatures.
  • Fig. 16 shows the representation of the state points of a co-electrolysis process with separate electrolyses and water quenching of the CO-rich synthesis gas. It shows the electrolytic decomposition of C0 2 (point 1) and H 2 0 (point 4) and the subsequent quenching with water.
  • Synthesis gas (item 6) mixed.
  • Fig. 17 is the representation of the state points of a co-electrolysis process with separate electrolysis and quenching of the CO-rich synthesis gas with cooled
  • Hydrogen shown It shows the quenching of the hot CO-containing gas with recuperatively cooled hydrogen.
  • the CO-containing gas formed (point 2) is quenched with cooled H 2 -rich gas (point 5).
  • the H 2 -rich gas (point 5) from the H 2 0-SOEC is previously cooled recuperative in a heat exchanger.
  • the resulting gas mixture (item 6) is cooled, and after the separation of the condensate, the finished synthesis gas is obtained (item 7).
  • Fig. 1 is a schematic representation of a procedural circuit of the RWGS
  • Figure 2 shows a possible procedural circuit of the co-electrolysis process.
  • Fig. 3 shows a RWGS process for the production of synthesis gas, in which to avoid
  • Soot formation after intercooling water vapor is mixed into the hot, to be cooled synthesis gas
  • Fig. 4 shows an RWGS process in which the steam is mixed before mixing into the
  • FIG. 5 shows a co-electrolysis process with steam mixing before gas cooling with preheating of the steam by process heat;
  • Figure 6 shows a co-electrolysis process with hydrogen surplus mode to avoid soot formation during gas cooling.
  • FIG. 7 shows an electrolysis process for the production of synthesis gas from water vapor and carbon dioxide with the aid of two separate electrolyses for water vapor and carbon dioxide in a first variant
  • Fig. 8 shows an electrolysis process for the production of synthesis gas from water vapor
  • Fig. 1 shows a schematic representation of a procedural circuit of the RWGS process.
  • feed gases for the RWGS process are carbon dioxide C0 2 , hydrogen H 2 , possibly residual gases from a Fischer Tropsch synthesis SPG, which unreacted
  • Synthesis gas components contains carbon monoxide and hydrogen and carbon dioxide and low hydrocarbons, and water vapor H 2 Og used.
  • the feed gas mixture 1 is called in the recuperator 2 against the approximately 900 to 950 ° C.
  • Preheated synthesis gas stream 6 and then fed as stream 3 to the electric power operated heater 4.
  • the gas mixture 3 is further heated and thereby fed so much heat that in the subsequent catalytic reactor 5, the endothermic reverse water gas shift reaction (RWGS reaction)
  • the about 900 to 950 ° C hot synthesis gas 6 is recuperatively cooled in the heat exchanger 2 against the heated feed gas 1 and then in operated with cooling water end cooler 7. During the cooling of the synthesis gas, water of reaction can condense out. The condensate 8 is discharged from the process.
  • the synthesis gas stream 6 is cooled less, which must be compensated by the final cooler 7.
  • the deposited in the heat exchanger 2 soot also clogs the gas channels in the heat exchanger.
  • the thus increasing flow pressure loss is measured by the differential pressure measurement 9 and must be compensated by a higher pressure of the supplied feed gas streams C0 2 , H 2 , SPG and H 2 Og. If this is not possible, the total quantity of feed gas must be reduced, which ultimately leads to a reduction in the output of the RWGS plant.
  • Fig. 2 shows a possible procedural circuit of the co-electrolysis process of the prior art.
  • the feed gases carbon dioxide C0 2 and water vapor H 2 Og are mixed and recuperatively cooled as gas mixture 100 in the heat exchanger 101 against the hot
  • Synthesis gas 107 preheated as far as possible.
  • the electrolytic decomposition is not complete and the synthesis gas 107 leaving the stack 105 is largely in chemical equilibrium, so that in the
  • the synthesis gas 107 which has a temperature of approximately 850 ° C., is first recuperatively cooled in the heat exchanger 101 against the feed gas mixture 100 to be heated and then in the final cooler 108 operated with cooling water. The resulting in the cooling by condensation of the residual steam in the synthesis gas condensate 109 is discharged from the process.
  • the cooled syngas SYG is supplied for subsequent use.
  • the electrolytically separated in the electrolysis stack 105 oxygen is on the anode side of the stack of purge air air preheated in the recuperator 201 against the cooled oxygen-air mixture 110 and then reheated in the electric heater 203 to about 850 ° C, removed and after cooling discharged in the recuperator 201 as exhaust gas EXG to the atmosphere.
  • the gas During the cooling of the synthesis gas 107 in the heat exchanger 101, the gas enters the soot area and soot is produced.
  • Electrolysis stacks 105 which can lead to breakage of individual cells and thus to performance losses and total failure of the co-electrolysis system.
  • Fig. 3 shows a RWGS process for the production of synthesis gas, in which, to avoid soot formation after an intermediate cooling water vapor H 2 0g.2 is mixed in the hot, to be cooled synthesis gas (Wasserdampfzumischung before the
  • Synthesis gas cooling without steam preheating (RWGS)
  • the steam comes from an external source and is in this variant before interference in the hot
  • the approximately 900 to 950 ° C hot synthesis gas 6 is first cooled in the recuperator 2.2 to a temperature of about 600 to 650 ° C.
  • the temperature of the intermediate cooling may only be so low that the state point of the cooled
  • Synthesis gas in the state diagram (Fig. 13) is still outside the Ruß meanses at the appropriate cooling temperature. So that no soot is still formed in the heat exchanger 2.2.
  • water vapor H 2 0g.2 is mixed in from an external source. Due to the water vapor mixing, the state point of the
  • Synthesis gas in the state diagram (Fig. 13) in the direction of water shifted in the direction of water shifted.
  • the synthesis gas-water vapor mixture 11 reaches the soot area, preferably at lower temperatures, where the kinetics no longer allow soot formation.
  • the resulting amount of condensate 8 is higher than in the prior art due to the Wasserdampfzumischung.
  • the water vapor mixture in the synthesis gas to be cooled is also without
  • Electric heater 4 thus needs more electric power to be used to the same
  • Fig. 4 therefore shows an RWGS process in which the steam is preheated by process heat before mixing into the intercooled synthesis gas and thus the exergy loss due to the steam mixture is lower (steam admixing before synthesis gas cooling with steam preheating (RWGS)).
  • the approximately 900 to 950 ° C hot synthesis gas stream 6 is first recooled as in the process Fig. 3 recuperative against the heated feed gas mixture in the heat exchanger 2.2 to about 600 to 650 ° C.
  • water vapor H 2 0g.2 is mixed from external sources, which was previously preheated in the recuperator 2.3 against the partial stream 12.2 of the synthesis gas - steam mixture 11.
  • the other partial stream 12.1 of the synthesis gas-steam mixture 11 is used for the first preheating stage of the feed gas mixture 1 in the heat exchanger 2.1.
  • recuperative cooled synthesis gas streams 13.1 and 13.2 are in the
  • Cooling chillers 7.1 and 7.2 cooled against cooling water to the desired final temperature.
  • the condensate streams 8.1 and 8.2 are removed from the process.
  • the water vapor mixture in the synthesis gas to be cooled can also be carried out without intermediate cooling of the synthesis gas before the steam mixture.
  • the steam mixture in the synthesis gas to be cooled to prevent soot formation during cooling is also in a co-electrolysis process for the production of
  • Fig. 5 shows a co-electrolysis process with steam mixing before the gas cooling with preheating of the steam by process heat (Wasserdampfzumischung before the
  • the approximately 850 ° C hot synthesis gas 107 is first cooled in the heat exchanger 101.2 to about 650 to 700 ° C. At this temperature, the gas mixture is not yet in the Ruß.
  • steam H 2 Og.2 is mixed from an external source, which was preheated in the heat exchanger 101.3 against a partial stream 114.2 of the steam-synthesis gas mixture 113.
  • the state point of the gas mixture 113 shifts in the direction of water and, during the further cooling in the heat exchangers 101. 1 and 101. 3, only reaches the soot area at a lower temperature. At this temperature, due to the kinetics of the soot formation reactions R1 and R2 and the short residence time of the gas mixture in the heat exchanger no soot is expected.
  • the second partial stream 114.1 of the steam-synthesis gas mixture 113 is used for the recuperative preheating of the feed gas mixture 100 in the heat exchanger 101.1.
  • the recuperatively cooled synthesis gas streams 115.1 and 115.2 are in the
  • control valve 117 In the control valve 117, the cooled synthesis gas streams 116.1 and 116.2 are combined again into the total flow SYG.
  • the water vapor mixture in the synthesis gas to be cooled is also without
  • Fig. 6 shows a co-electrolysis process with hydrogen excess mode for
  • the separated hydrogen 118 is typically depressurized by the gas separation device 119 and the synthesis gas is supplied to a synthesis which is operated under pressure
  • the total gas stream 116 is increased in pressure prior to gas separation with the compressor 120.
  • the compressor 120 may also be in the separated hydrogen stream 118.
  • Synthesis gas flow SYG measured H 2 - and CO concentrations is used, the control valve 123, which leads a bypass flow 124 to the gas separation device 119.
  • Fig. 7 is an electrolysis process for the production of synthesis gas from water vapor and carbon dioxide by means of two separate electrolyses for water vapor and
  • Carbon dioxide shown (separate H 2 0 and C0 2 electrolysis and quenching of CO rich gas with water).
  • the CO-containing product stream from the C0 2 electrolysis is quenched with water and thus rapidly cooled, which suppresses or prevents soot formation during cooling.
  • Carbon dioxide C0 2 is preheated in the heat exchanger 101.3 against the partial flow 126.2 of the hot oxygen-air mixture 110 and then heated in the electric heater 103.2 to an inlet temperature of about 850 ° C in the stack 105.2.
  • the hot carbon dioxide 104.2 is decomposed by means of electric energy 106.2 into carbon monoxide and oxygen.
  • the decomposition of the C0 2 is not complete, so that in the exiting gas 107.2 after the stack 105.2 in addition to CO still C0 2 is included.
  • the about 850 ° C hot CO-C0 2 mixture 107.2 is cooled in the quencher 127 by injecting water 128 shock. The rapid cooling prevents soot formation. If, however, little soot is formed, it is washed out of the gas by the atomized water and ends up in the quench 127 of the quench, from where it is separated as
  • Mud water 129 withdrawn and fed to a further treatment.
  • the quench water also accumulating in the sump passes through an overflow in the subsequent cooler 130.
  • a partial flow of the cooled water 131 is recirculated by means of the pump 132 and fed as quench water 128 to the quencher 127 again.
  • a portion of the water is discharged as wastewater ABW.
  • the additional water H 2 Of serves to compensate for water losses in Quenchingernikank.
  • the steam H 2 Og is preheated in the heat exchanger 101.1 against the hot, to be cooled H 2 - H 2 0 mixture 107.1 and then preheated by means of the electric heater 103.1 to inlet temperature of about 850 ° C in the stack 105.1.
  • the electrolytic decomposition of the hot water vapor 104.1 into hydrogen and oxygen takes place with the aid of electric energy 106.1.
  • the decomposition of the water vapor is not complete, so that in the exiting gas 107.1 after the stack 105.1 next to hydrogen nor water vapor is included.
  • the cooled in the heat exchanger 101.1 H 2 -H 2 0 mixture 133.1 is mixed with the cooled in quencher 127 CO-C0 2 mixture 133.2, which is saturated by quenching with water vapor, and fed as a gas mixture 134 operated with cooling water end cooler 108 , After final cooling, the finished synthesis gas SYG reaches the subsequent synthesis. The resulting in the cooling condensate 109 is discharged from the process.
  • the in the stacks 105.1 and 105.2 electrolytically split off from C0 2 and H 2 0 oxygen is scavenged air, in the heat exchanger 201 against the second partial flow 126.1 of about 850 ° C hot air-0 2 mixture 110, resulting from the Streams 110.1 and 110.2 composed of the stacks 105.1 and 105.2, preheated.
  • the purge air is divided into stacks 105.1 and 105.2 and heated in the electric heaters 203.1 and 203.2 to an inlet temperature of about 850 ° C.
  • exhaust gas air-0 2 mixture
  • control valve 123 temperature regulated 135.1, 135.2
  • Fig. 8 is an electrolysis process for the production of synthesis gas from water vapor and carbon dioxide by means of two separate electrolyses for water vapor and
  • Carbon dioxide (separate H 2 O and CQ 2 electrolysis and quenching of the CO containing gas with cold hydrogen).
  • the carbon monoxide-containing product stream from the C0 2 - electrolysis is quenched with cooled H 2 -rich gas from the H 2 0 electrolysis and thus cooled rapidly, which suppresses or prevents soot formation during cooling.
  • Carbon dioxide C0 2 is preheated in the heat exchanger 101.3 against the partial flow 126.2 of the hot exhaust gas 110 and then heated in the electric heater 103.2 to an inlet temperature of about 850 ° C in the stack 105.2.
  • the hot carbon dioxide 104.2 is decomposed by means of electric energy 106.2 into carbon monoxide and oxygen.
  • the decomposition of the C0 2 is not complete, so that in the exiting gas 107.2 after the stack 105.2 in addition to CO still C0 2 is included.
  • the about 850 ° C hot CO-C0 2 mixture 107.2 is cooled in the gas quencher 136 by mixing cold H 2 -rich gas 137 shock. The rapid cooling prevents soot formation.
  • the steam H 2 Og is preheated in the heat exchanger 101.1 against the hot, to be cooled H 2 - H 2 0 mixture 107.1 and then preheated by means of the electric heater 103.1 to inlet temperature of about 850 ° C in the stack 105.1.
  • the electrolytic decomposition of the hot water vapor 104.1 into hydrogen and oxygen takes place with the aid of electric energy 106.1.
  • the decomposition of the water vapor is not complete, so that in the exiting gas 107.1 after the stack 105.1 next to hydrogen nor water vapor is included.
  • Condensate 109 is removed from the process.
  • the gas 139 is cooled in the second cooling cooler 108 operated with cooling water and finished
  • Synthesis gas SYG supplied to the subsequent synthesis process Synthesis gas SYG supplied to the subsequent synthesis process.
  • the split off in the stacks 105.1 and 105.2 electrolytically from C0 2 and H 2 0 oxygen is scavenged air, in the heat exchanger against the second partial flow 126.1 of about 850 ° C hot air-0 2 mixture 110 resulting from the streams 110.1 and 110.2 composed of the stacks 105.1 and 105.2, preheated.
  • the purge air is divided into stacks 105.1 and 105.2 and heated in the electric heaters 203.1 and 203.2 to an inlet temperature of about 850 ° C.
  • exhaust gas air-0 2 mixture
  • control valve 123 temperature regulated 135.1, 135.2
  • H 2 is hydrogen
  • gas separation co-electrolysis e.g., membrane

Abstract

La présente invention concerne un procédé pour éviter et/ou réduire la quantité de suie pour éviter et/ou réduire la quantité de suie à l'intérieur d'un dispositif produisant un gaz de synthèse et/ou un gaz contenant du CO à partir des gaz d'alimentation tels que le dioxyde de carbone, la vapeur d'eau, l'hydrogène et/ou un gaz de queue hydrocarboné ainsi que l'énergie électrique dans les processus de réaction RWGS, les électrolyses pour la décomposition électrochimique du dioxyde de carbone et/ou de la vapeur d'eau, les procédés de reformage et/ou les processus de production de gaz de synthèse avec au moins une unité de production de gaz, un empilement électrolytique et/ou une combinaison dispositif de chauffage-réacteur afin de réaliser une réaction RWGS et au moins avec un segment de refroidissement/récupérateur pour le gaz contenant du CO et/ou du gaz de synthèse. L'invention concerne également un système pour éviter et/ou réduire la quantité de suie.
EP18730971.1A 2017-06-12 2018-06-11 Procédé et système pour éviter et/ou réduire la quantité de suie Pending EP3638620A1 (fr)

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EP17175569.7A EP3415466A1 (fr) 2017-06-12 2017-06-12 Procédé et système de réduction de suie et/ou destinés à éviter la suie et procédé et système d'élimination de suie dans des voies de refroidissement et récupérateurs
PCT/DE2018/100553 WO2018228642A1 (fr) 2017-06-12 2018-06-11 Procédé et système pour éviter et/ou réduire la quantité de suie

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EP18730970.3A Pending EP3638619A1 (fr) 2017-06-12 2018-06-11 Procédé et système d'élimination de la suie dans des sections de refroidissement et des récupérateurs
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EP18730970.3A Pending EP3638619A1 (fr) 2017-06-12 2018-06-11 Procédé et système d'élimination de la suie dans des sections de refroidissement et des récupérateurs

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US20240116756A1 (en) * 2022-10-06 2024-04-11 Air Products And Chemicals, Inc. Process and System for Water-Gas Shift Conversion of Synthesis Gas with High CO Concentration

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CA3067090C (fr) 2023-02-21
AU2018283056A1 (en) 2019-12-19
CA3067090A1 (fr) 2018-12-20
WO2018228641A1 (fr) 2018-12-20
AU2018283056B2 (en) 2020-07-16
ZA201906574B (en) 2020-08-26
EP3638619A1 (fr) 2020-04-22
US11612872B2 (en) 2023-03-28
US20200179897A1 (en) 2020-06-11

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