WO2013135657A1 - Procédé de production de gaz de synthèse en fonctionnement alterné entre deux types de fonctionnements - Google Patents

Procédé de production de gaz de synthèse en fonctionnement alterné entre deux types de fonctionnements Download PDF

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Publication number
WO2013135657A1
WO2013135657A1 PCT/EP2013/054943 EP2013054943W WO2013135657A1 WO 2013135657 A1 WO2013135657 A1 WO 2013135657A1 EP 2013054943 W EP2013054943 W EP 2013054943W WO 2013135657 A1 WO2013135657 A1 WO 2013135657A1
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heating
group
reaction
threshold value
fluid
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German (de)
English (en)
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Leslaw Mleczko
Vanessa GEPERT
Alexander Karpenko
Emanuel Kockrick
Albert TULKE
Daniel Gordon Duff
Alexandra GROSSE BÖWING
Daniel Wichmann
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Bayer Intellectual Property Gmbh
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Publication of WO2013135657A1 publication Critical patent/WO2013135657A1/fr

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    • B01J2219/2416—Additional heat exchange means, e.g. electric resistance heater, coils
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    • C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
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Definitions

  • the present invention relates to a process for the production of synthesis gas, comprising the steps of providing a flow reactor, setting thresholds, comparing energy prices and / or energy composition with respect to regenerative sources, and a choice between the modes of dry reforming / reverse water gas shift reaction on the one hand and catalytic Partial oxidation on the other hand.
  • synthesis gas is produced by steam reforming of methane. Due to the high heat demand of the reactions involved, they are carried out in externally heated reformer tubes. Characteristic of this method is the limitation by the reaction equilibrium, a heat transport limitation and especially the pressure and temperature limitation of the reformer tubes used (nickel-based steels). Temperature and pressure side results in a limitation to a maximum of 900 ° C at about 20 to 40 bar.
  • An alternative method is autothermal reforming.
  • a portion of the fuel is burned by the addition of oxygen within the reformer, so that the reaction gas is heated and the expiring endothermic reactions are supplied with heat.
  • DE 10 2007 022 723 A1 and US 2010/0305221 describe a process for the production and conversion of synthesis gas, which is characterized in that it has a plurality of different operating states which essentially comprise the alternating (i) daytime operation and (ii) nighttime operation where the day-to-day operation (i) mainly comprises dry reforming and steam reforming with the supply of regenerative energy and night operation (ii) mainly the partial oxidation of hydrocarbons and wherein the synthesis gas produced is used to produce value products.
  • US 2007/003478 Al discloses the production of synthesis gas with a combination of steam reforming and oxidation chemistry. The process involves the use of solids to heat the hydrocarbon feed and cool the gaseous product.
  • WO 2007/042279 AI deals with a reformer system with a reformer for the chemical reaction of a hydrocarbon-containing fuel in a hydrogen gas-rich reformate gas, and electric heating means by which the reformer heat energy for producing a reaction temperature required for the feed can be supplied, wherein the reformer system further comprises a capacitor has, which can supply the electric heating means with electric current.
  • WO 2004/071947 A2 / US 2006/0207178 AI relate to a system for the production of hydrogen, comprising a reformer for generating hydrogen from a hydrocarbon fuel, a compressor for compressing the generated hydrogen, a renewable energy source for converting a renewable resource into electrical Energy for driving the compressor and a storage device for storing the hydrogen from the compressor.
  • the object of the present invention is to provide such a method.
  • it has set itself the task of specifying a method for the production of synthesis gas, which is suitable for alternating operation between two different modes of operation.
  • a process for the production of synthesis gas comprising the steps: a) providing a flow reactor, which is arranged to react a fluid comprising reactants, wherein the reactor comprises at least one heating level, which is electrically heated by means of one or more heating elements, and wherein the heating level can be traversed by the fluid and at least one heating element Catalyst is arranged and is heated there; b) setting a threshold value S l for the costs of the electrical energy available for the flow reactor and / or a threshold value S2 for the relative proportion of electrical energy from regenerative sources of the electrical energy available for the flow reactor; and c) comparing the costs of the electrical energy available for the flow reactor with the threshold value Sl and / or the relative proportion of electrical energy from regenerative sources of the electrical energy available for the flow reactor with the threshold value S2; d) reaction of carbon dioxide with hydrocarbons, water and / or hydrogen in the flow reactor, wherein at least carbon monoxide is formed as product, with electrical heating by
  • the first threshold Sl relates to the electricity costs for the reactor, in particular the costs for electrical heating of the reactor by the heating elements in the heating levels. Here it can be determined up to which height the electric heating is still economically reasonable.
  • the second threshold S2 relates to the relative proportion of electrical energy from regenerative sources available to the reactor and, in particular, to the electrical heating of the reactor by the heating elements in the heating levels.
  • the relative proportion is in this case based on the total electrical energy of the electric current available for the flow reactor and can of course vary over time. Examples of regenerative sources from which electrical energy can be obtained are wind, solar, geothermal, wave and hydro.
  • the relative share can be determined by providing information to the energy supplier. For example, stand up If a factory site has its own regenerative energy sources such as solar installations or wind turbines, then this relative energy proportion can also be specified via performance monitoring.
  • the threshold value S 1 can be understood, for example, as a price upper limit
  • the threshold value S2 can be understood as a requirement to use renewable energies to the greatest possible extent.
  • S2 may mean that from a proportion of 5%, 10%, 20% or 30% of electrical energy from renewable sources, the electrical heating of the reactor should take place.
  • the flow reactor is operated so that, for example, run a dry reforming reaction, steam reforming reaction or a reverse water gas shift reaction.
  • the hydrocarbons involved are preferably alkanes, alkenes, alkynes, alkanols, alkenols and / or alkynols.
  • alkanes methane is particularly suitable, among the alkanols methanol and / or ethanol are preferred.
  • Reverse water gas shift reaction C0 2 + H 2 * ⁇ CO + H 2 0 If the target / actual comparison shows that electrical energy is too expensive and / or too much energy from non-renewable sources is needed, Thus, the operating mode of the flow reactor is changed over and a partial oxidation takes place. It is reproduced using the example of methane.
  • the exothermic partial oxidation gives the required thermal energy and continues to produce syngas.
  • production can be continued in the same reactor.
  • the combustion of hydrogen can be used. It is also possible that the combustion of hydrogen in the rWGS reaction by metering of 0 2 in the educt gas (ideally a locally distributed or lateral addition) takes place, as well as possible that hydrogen-rich residual gases (for example, PSA exhaust gas), as they may be incurred in the purification of the synthesis gas, recycled and burned together with O2, which then the process gas is heated.
  • hydrogen-rich residual gases for example, PSA exhaust gas
  • An advantage of the oxidative mode of operation is that soot deposits formed by dry reforming or steam reforming can be removed and thus the catalyst used can be regenerated. Moreover, it is possible to regenerate passivation layers, the heating conductor or other metallic internals in order to increase the service life.
  • endothermic reactions are heated from the outside through the walls of the reaction tubes. Opposite is the autothermal reforming with 02 addition.
  • the endothermic reaction can be efficiently internally supplied with heat via an electrical heating within the reactor (the undesired alternative would be electrical heating via radiation through the reactor wall). This type of reactor operation is particularly economical if the excess supply resulting from the expansion of renewable energy sources can be used cost-effectively.
  • the process according to the invention provides for the DR, SMR, RWGS and POX reactions to proceed in the same reactor.
  • a mixed operation is expressly provided.
  • One of the advantages of this approach is the gradual onset of each other's reaction, for example, by continuously reducing hydrogen supply while increasing the supply of methane, or by continuously increasing hydrogen supply while reducing methane feed.
  • FIG. 1 shows schematically a flow reactor in an expanded representation.
  • the flow reactor comprises a plurality of heating levels seen in the flow direction of the fluid, which are electrically heated by heating elements and wherein the heating levels are flowed through by the fluid, wherein at least one heating element, a catalyst is arranged and is heated there, wherein Furthermore, at least once an intermediate level between two heating levels is arranged and wherein the intermediate level is also traversed by the fluid.
  • the in FIG. 1 schematically shown flow reactor used according to the invention is flowed through by a fluid comprising reactants from top to bottom, as shown by the arrows in the drawing.
  • the fluid may be liquid or gaseous and may be single-phase or multi-phase.
  • the fluid is gaseous. It is conceivable that the fluid contains only reactants and reaction products, but also that additionally inert components such as inert gases are present in the fluid.
  • the reactor has a plurality of (four in the present case) heating levels 100, 101, 102, 103, which are electrically heated by means of corresponding heating elements 110, 111, 112, 113.
  • the heating levels 100, 101, 102, 103 are flowed through by the fluid in the operation of the reactor and the heating elements 1 10, 11 1, 1 12, 1 13 are contacted by the fluid.
  • At least one heating element 110, 111, 112, 113, a catalyst is arranged and is heated there.
  • the catalyst may be directly or indirectly connected to the heating elements 110, 11 1, 12, 13, so that these heating elements represent the catalyst support or a support for the catalyst support.
  • the heat supply of the reaction takes place electrically and is not introduced from the outside by means of radiation through the walls of the reactor, but directly into the interior of the reaction space. It is realized a direct electrical heating of the catalyst.
  • Thermistor alloys such as FeCrAl alloys are preferably used for the heating elements 110, 111, 112, 113.
  • electrically conductive Si-based materials particularly preferably SiC.
  • This has the effect of homogenizing the fluid flow.
  • additional catalyst can be present in one or more intermediate levels 200, 20 1, 202 0 of the further insulation elements in the reactor. Then an adiabatic reaction can take place. If necessary, the intermediate levels can act as a flame barrier, especially in the POX reaction.
  • Said at least one intermediate ceramic layer is preferably supported by a ceramic or metallic support frame and / or a ceramic or metallic support plane.
  • a ceramic or metallic support frame and / or a ceramic or metallic support plane When using FeCrAl thermistors, the fact can be exploited that the material forms an AhC protective layer as a result of the effect of temperature in the presence of air / oxygen.
  • This passivation layer can serve as a basecoat of a washcoat, which acts as a catalytically active coating.
  • the direct resistance heating of the catalyst or the heat supply of the reaction is realized directly through the catalytic structure. It is also possible, when using other thermistor, the formation of other protective layers such as Si-OC systems.
  • the pressure in the reactor can take place via a pressure-resistant steel jacket.
  • suitable ceramic insulation materials it can be achieved that the pressure-bearing steel is exposed to temperatures of less than 200 ° C and, if necessary, less than 60 ° C.
  • the electrical connections are shown in FIG. 1 only shown very schematically. They can be performed in the cold area of the reactor within an insulation to the ends of the reactor or laterally from the heating elements 1 10, 1 1 1, 1 12, 1 13 performed so that the actual electrical connections can be provided in the cold region of the reactor ,
  • the electrical heating is done with direct current or alternating current.
  • heating elements 1 10, 1 1 1, 1 12, 1 13 are arranged, which are constructed in a spiral, meandering, lattice-shaped and / or reticulated.
  • At least one heating element 110, 11 1, 1 12, 1 13 one of the remaining heating elements 1 10, 1 1 1, 1 12, 1 13 different amount and / or type of catalyst is present.
  • the heating elements 110, 111, 112, 113 are arranged so that they can each be electrically heated independently of each other.
  • the individual heating levels can be individually controlled and regulated.
  • In the reactor inlet area can be dispensed with a catalyst in the heating levels as needed, so that only the heating and no reaction takes place in the inlet area. This is particularly advantageous in terms of starting the reactor. If the individual heating levels 100, 101, 102, 103 differ in power input, catalyst charge and / or type of catalyst, a temperature profile adapted for the respective reaction can be achieved.
  • the (for example ceramic) intermediate levels 200, 201, 202 or their contents 210, 21 1, 212 comprise a material resistant to the reaction conditions, for example a ceramic foam. They serve for mechanical support of the heating levels 100, 101, 102, 103 and for mixing and distribution of the gas stream. At the same time an electrical insulation between two heating levels is possible.
  • the material of the content 210, 21 1, 212 of an intermediate level 200, 201, 202 comprises oxides, carbides, nitrides, phosphides and / or borides of aluminum, silicon and / or zirconium. An example of this is SiC. Further preferred is cordierite.
  • the intermediate level 200, 201, 202 may include, for example, a loose bed of solids. These solids themselves may be porous or solid, so that the fluid flows through gaps between the solids. It is preferred that the material of the solid bodies comprises oxides, carbides, nitrides, phosphides and / or borides of aluminum, silicon and / or zirconium. An example of this is SiC. Further preferred is cordierite.
  • the intermediate plane 200, 201, 202 comprises a one-piece porous solid.
  • the fluid flows through the intermediate plane via the pores of the solid. This is shown in FIG. 1 shown.
  • Preference is given to honeycomb monoliths, as used for example in the exhaust gas purification of internal combustion engines.
  • one or more of the intermediate levels are voids.
  • the average length of a heating level 100, 101, 102, 103 is viewed in the direction of flow of the fluid and the average length of an intermediate level 200, 201, 202 in the direction of flow of the fluid is in a ratio of> 0.01: 1 to ⁇ 100: 1 to each other. Ratios of> 0.1: 1 to ⁇ 10: 1 or 0.5: 1 to ⁇ 5: 1 are even more advantageous.
  • Suitable catalysts may, for example, be selected from the group:
  • A, A 'and A are independently selected from the group: Mg, Ca, Sr, Ba, Li, Na, K, Rb, Cs, Sn, Sc, Y, La, Ce, Pr, Nd, Pm, Sm , Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Tl, Lu, Ni, Co, Pb, Bi and / or Cd; and B, B 'and B "are independently selected from the group: Cr, Mn, Fe, Bi, Cd, Co, Cu, Ni, Sn, Al, Ga, Sc, Ti, V, Nb, Ta, Mo, Pb , Hf, Zr, Tb, W, Gd, Yb, Mg, Li, Na, K, Ce and / or Zn; and
  • A, A 'and A are independently selected from the group: Mg, Ca, Sr, Ba, Li, Na, K, Rb, Cs, Sn, Sc, Y, La, Ce, Pr, Nd, Sm, Eu , Gd, Tb, Dy, Ho, Er, Tm, Yb, Tl, Lu, Ni, Co, Pb and / or Cd; and B is selected from the group: Cr, Mn, Fe, Bi, Cd, Co, Cu , Ni, Sn, Al, Ga, Sc, Ti, V, Nb,
  • B ' is selected from the group: Re, Ru, Rh, Pd, Os, Ir and / or Pt;
  • B is selected from the group: Cr, Mn, Fe, Bi, Cd, Co, Cu, Ni, Sn, Al, Ga, Sc, Ti, V, Nb, Ta, Mo, Pb, Hf, Zr, Tb, W, Gd, Yb, Mg, Cd and / or Zn, and 0 ⁇ w ⁇ 0.5, 0 ⁇ x ⁇ 0.5, 0 ⁇ y ⁇ 0.5, 0 ⁇ z ⁇ 0.5 and -l ⁇ delta ⁇ 1;
  • Ml and M2 are independently selected from the group: Re, Ru, Rh, Ir, Os, Pd and / or Pt;
  • M3 is selected from the group: Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and / or Lu.
  • M is selected from the group: Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Zn, Cu , Ag and / or Au; and
  • L is selected from the group: Na, K, Rb, Cs, Mg, Ca, Sr, Ba, Sc, Y, Sn, Pb, Mn, In, Tl, La, Ce, Pr, Nd, Sm, Eu, Gd , Tb, Dy, Ho, Er, Tm, Yb and / or Lu; and
  • Ml and M2 are independently selected from the group: Cr, Mn, Fe, Co, Ni, Re, Ru, Rh, Ir, Os, Pd, Pt, Zn, Cu, La, Ce, Pr, Nd, Sm, Eu , Gd, Tb, Dy, Ho, Er, Tm, Yb, and / or Lu; and
  • a and B are independently selected from the group: Be, Mg, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Y, Zr, Nb, Mo, Hf, Ta, W, La, Ce , Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and / or Lu; and or
  • reaction products includes the catalyst phases present under reaction conditions. Preferred are for:
  • an electric heating of at least one of the heating elements 110, 11 1, 1 12, 113 takes place in the reactor provided. This can, but does not have to be, carried out in advance of the passage of a reactant comprising the fluid through the flow reactor with at least partial reaction of the reactants of the fluid ,
  • the reactor can be modular.
  • a module may include, for example, a heating level, an insulation level, the electrical contact and the corresponding further insulation materials and thermal insulation materials.
  • the individual heating elements 110, 111, 112, 113 are operated with a respective different heating power.
  • the reaction temperature in the reactor is at least in places> 700 ° C to ⁇ 1300 ° C. More preferred ranges are> 800 ° C to ⁇ 1200 ° C and> 900 ° C to ⁇ 1100 ° C.
  • the average (mean) contact time of the fluid to a heating element 110, 111, 112, 113 may be, for example,> 0.01 seconds to ⁇ 1 second and / or the average contact time of the fluid to an intermediate level 110, 111, 112, 113 may be, for example > 0.001 seconds to ⁇ 5 seconds.
  • Preferred contact times are> 0.005 to ⁇ 1 second, more preferably> 0.01 to ⁇ 0.9 seconds.
  • the reaction can be carried out at a pressure of> 1 bar to ⁇ 200 bar.
  • the pressure is> 2 bar to ⁇ 50 bar, more preferably> 10 bar to ⁇ 30 bar.
  • f) a desired H 2 / CO ratio in the synthesis gas is determined and g) the reaction of carbon dioxide with hydrocarbons, water and / or hydrogen in the flow reactor, at least carbon monoxide being formed as product, with electric heating by one or more heating elements (1 10, 1 1 1, 1 12, 1 13) is carried out when the desired ratio of H 2 / CO is exceeded; and h) the reaction of hydrocarbons with oxygen in the flow reactor, wherein as products at least carbon monoxide and hydrogen are formed, is carried out when the desired ratio of H2 / CO is exceeded; with the following exception: a change from the reaction of carbon dioxide with hydrocarbons, at least carbon monoxide being formed as product, for the reaction of hydrocarbons with oxygen, forming at least carbon monoxide and hydrogen as products, then takes place
  • the H 2 / CO ratio changes from 1: 1 to 2: 1 when changing from CC reforming to POX. Modifications by adding H 2 O or CO 2 to the SMR are also possible. When changing from Dry Reforming to POX, however, the H 2 / CO ratio changes from 1: 1 to 2: 1.
  • the main target product may be CO or H 2 .
  • the characteristic value Sl has fallen below and / or the characteristic value S2 has been exceeded.
  • the endothermic operation that is, steam reforming or dry reforming, wherein in addition to CO2 as Cl source is used, which is reflected in a saving of methane, preferred.
  • dry reforming two moles of CO and two moles of H2 are obtained per mole of methane.
  • the educt ratio of CO2 / CH4 is> 1.25.
  • the CO2 present in the product gas is separated off in subsequent process steps and returned to the reactor.
  • the mode of operation is changed over from the endothermic operation to the exothermic operation.
  • methane is fed with 02 to the reactor.
  • CO2 can be further added during the switching phase and used as a kind of inert component until the POX reaction is stabilized and a new stationary state is reached.
  • the CO 2 separated off in the succeeding steps can be temporarily stored in order to be used as reactant at the start of the endothermic reaction.
  • the reactant streams or the throughput of methane and oxygen are adjusted so that a constant amount of CO or H2 amount is available for subsequent processes.
  • the target product is CO.
  • the characteristic value S l has fallen below and / or the characteristic value S2 has been exceeded.
  • endothermic operation that is, performance of the rWGS reaction using CO2 as the Cl source, is preferred.
  • one mole of CO and one mole of water will be present per mole of CO2.
  • the educt ratio of H2 / CO2 is> 1.25.
  • the CO2 present in the product gas is separated off in subsequent process steps and returned to the reactor.
  • the characteristic value Sl is exceeded and / or the characteristic value S2 is undershot, the mode of operation is changed over from the endothermic operation to the exothermic operation.
  • methane is fed with O 2 to the reactor.
  • CO2 can be further added during the switching phase and used as a kind of inert component until the POX reaction is stabilized and a new stationary state is reached.
  • Part of the hydrogen produced during POX operation can be cached and used to operate the rWGS reaction.
  • the electrical heating elements can be used in the region of the reactor inlet for the starting process.
  • a rapid heating of the reactant stream is possible, which reduces coking when carrying out the endothermic reforming reactions and, when carrying out the POX, allows a locally defined ignition of the reaction and thus enables safe reactor operation.

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Abstract

La présente invention concerne un procédé qui consiste à préparer un réacteur à circulation conçu pour permettre la réaction d'un fluide contenant des réactifs, à déterminer une valeur seuil S1 pour les coûts de l'énergie électrique mise à disposition pour le réacteur à circulation et/ou une valeur seuil S2 pour la proportion relative d'énergie électrique provenant de sources d'énergie renouvelable de l'énergie électrique mise à disposition pour le réacteur à circulation; puis à comparer les coûts de l'énergie électrique mise à disposition pour le réacteur à circulation à la valeur seuil S1 et/ou la proportion relative d'énergie électrique provenant de sources d'énergie renouvelable de l'énergie électrique mise à disposition pour le réacteur à circulation à la valeur seuil S2. Des réactions de reformage à sec ou de gaz à l'eau inverse (RWGS) ont lieu lorsque la valeur est inférieure à la valeur seuil S1 et/ou supérieure à la valeur seuil S2. Des réactions d'oxydation partielle catalytique ont lieu lorsque la valeur est supérieure à la valeur seuil S1 et/ou inférieure à la valeur seuil S2.
PCT/EP2013/054943 2012-03-13 2013-03-12 Procédé de production de gaz de synthèse en fonctionnement alterné entre deux types de fonctionnements WO2013135657A1 (fr)

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WO2023089184A1 (fr) * 2021-11-22 2023-05-25 Catagen Limited Système de traitement de fluide destiné à des systèmes d'alimentation en énergies renouvelables

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EP0913357A1 (fr) * 1997-10-28 1999-05-06 Ngk Insulators, Ltd. Dispositif de reformage et sa méthode de fonctionnement
DE10023410A1 (de) * 2000-05-12 2001-11-15 Linde Gas Ag Verfahren zur Erzeugung eines CO- und H2-haltigen Behandlungsgases für die Wärmebehandlung von metallischem Gut, Gasgenerator und Wärmebehandlungsanlage
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WO2004071947A2 (fr) 2003-02-06 2004-08-26 Ztek Corporation Systeme de reformage d'un hydrogene utilisant une energie renouvelable
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US20070003478A1 (en) 2005-06-29 2007-01-04 Becker Christopher L Synthesis gas production and use
WO2007042279A1 (fr) 2005-10-13 2007-04-19 Bayerische Motoren Werke Aktiengesellschaft Systeme reformeur comprenant des dispositifs de chauffage electriques
DE102007022723A1 (de) 2007-05-11 2008-11-13 Basf Se Verfahren zur Herstellung von Synthesegas
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DE10023410A1 (de) * 2000-05-12 2001-11-15 Linde Gas Ag Verfahren zur Erzeugung eines CO- und H2-haltigen Behandlungsgases für die Wärmebehandlung von metallischem Gut, Gasgenerator und Wärmebehandlungsanlage
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