US20110132770A1 - Process for producing compounds of the cxhyoz type by reduction of carbon dioxide (co2) and/or carbon monoxide (co) - Google Patents

Process for producing compounds of the cxhyoz type by reduction of carbon dioxide (co2) and/or carbon monoxide (co) Download PDF

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Publication number
US20110132770A1
US20110132770A1 US12/992,740 US99274009A US2011132770A1 US 20110132770 A1 US20110132770 A1 US 20110132770A1 US 99274009 A US99274009 A US 99274009A US 2011132770 A1 US2011132770 A1 US 2011132770A1
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steam
membrane
cathode
anode
equal
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Béatrice Sala
Olivier Lacroix
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Areva SA
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Areva SA
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    • 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
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/20—Processes
    • C25B3/25—Reduction

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  • the present invention relates to a process for producing compounds of the C x H y O z type, particularly with x>1; y is between 0 and 2x+2 and z is between 0 and 2 ⁇ , by reduction of carbon dioxide (CO 2 ) and/or carbon monoxide (CO), particularly from very reactive hydrogen species generated by water electrolysis.
  • CO 2 carbon dioxide
  • CO carbon monoxide
  • One of the main problems with this synthetic pathway is that it produces, as by-products, significant quantities of CO 2 -type greenhouse gases. In fact, 8 to 10 tons of CO 2 are released to produce 1 ton of hydrogen.
  • the energy necessary for this transformation would be electricity, for example of nuclear origin, and in particular that from reactors such as HTR “High Temperature Reactor” type nuclear reactors or EPR (registered trademark) European pressurized water reactors.
  • a promising path for industrial hydrogen production is the technique known as steam electrolysis, for example at high temperature (EHT), at medium temperature, typically over 200° C., or even at an intermediate temperature of between 200° C. and 1000° C.
  • EHT high temperature
  • medium temperature typically over 200° C.
  • intermediate temperature typically between 200° C. and 1000° C.
  • an electrolyte capable of carrying O 2 ⁇ ions and operating at temperatures that are generally between 750° C. and 1000° C. is utilized.
  • FIG. 1 schematically represents an electrolyser 1 comprising a ceramic membrane 2 , conductor of O 2 ⁇ ions, ensuring the electrolyte function separating an anode 3 and a cathode 4 .
  • the O 2 ⁇ ions more precisely the oxygen vacancies (V o .. ), migrate through electrolyte 2 to form oxygen O 2 at the surface of anode 3 , electrons e being released according to the oxidation reaction:
  • the first process enables, from the output of the electrolyzer 1 , oxygen—anode compartment—and hydrogen mixed with steam—cathode compartment—to be generated.
  • an electrolyte capable of carrying the protons and operating at lower temperatures than those required for the first process described above, generally between 200° C. and 800° C., is utilized.
  • FIG. 2 schematically represents an electrolyzer 10 comprising a proton-conducting ceramic membrane 11 ensuring the electrolyte function separating an anode 12 and a cathode 13 .
  • H + ions or OH o . Kroger-Vink notation migrate through the electrolyte 11 to form hydrogen H 2 at the surface of cathode 13 according to the equation:
  • this process provides, from the output of electrolyzer 10 , pure hydrogen—cathode compartment—and oxygen mixed with steam—anode compartment.
  • H 2 passes by the formation of intermediate compounds that are hydrogen atoms adsorbed at the surface of the cathode with variable energies and degrees of interaction and/or radical hydrogen atoms H • (or H Electrode x in Kroger-Vink notation).
  • these species are highly reactive, they usually recombine to form hydrogen H 2 according to the equation:
  • the present invention aims to reduce the quantity of existing carbon dioxide, for example by recycling this carbon dioxide in the form of compounds usable in the chemistry field or in the energy production field.
  • the invention proposes a process for electrolyzing water steam injected under pressure into an anode compartment of an electrolyzer provided with a proton-conducting membrane made of a material enabling protonated species to be incorporated into this membrane under steam, oxidation of the water injected in steam form taking place at the anode so as to generate protonated species in the membrane that migrate within this same membrane and are reduced at the surface of the cathode in the form of reactive hydrogen atoms capable of reducing carbon dioxide CO 2 and/or carbon monoxide CO, said process comprising the following steps:
  • reactive hydrogen atoms is understood to refer to hydrogen atoms adsorbed at the surface of the cathode with variable energies and degrees of interaction and/or radical hydrogen atoms H • (or H Electrode x in Kroger-Vink notation).
  • the invention results from the observation that the second process described above generates highly reactive hydrogen at the electrolyzer cathode (particularly hydrogen atoms adsorbed at the surface of the electrode and/or radical hydrogen atoms).
  • Electrode x are formed at the surface of the cathode according to the reaction:
  • the highly reactive hydrogen H Electrode x reacts with the carbon compounds on the electrode to give reduced carbon dioxide and/or carbon monoxide compounds of the C x H y O z type with x>1; y is between 0 and 2x+2 and z is between 0 and 2x.
  • these compounds are paraffins C n H 2 n + 2, olefins C 2n H 2n , alcohols C n H 2n+2 OH or C n H 2n ⁇ 1 OH, aldehydes and ketones C n H 2n O, acids C n ⁇ 1 H 2n+1 with n>1.
  • the invention thus enables steam to be electrolyzed with the joint carbon dioxide and/or carbon monoxide electroreduction as described subsequently.
  • the invention also relates to a steam electrolysis device for electrolyzing water steam introduced under pressure into an anode compartment of an electrolyzer provided with a proton-conducting membrane, made of a material enabling the injection of protonated species into this membrane under steam after oxidation, comprising:
  • the device according to the invention may also present one or more of the characteristics below, considered individually or according to all technically possible combinations:
  • FIG. 3 schematically and in a simplified manner represents an embodiment of an electrolysis device for the production of hydrogen implementing the joint CO 2 and/or CO electroreduction process according to the invention.
  • This electrolysis device has a structure similar to that of the device from FIG. 2 . Thus, it comprises:
  • the device also comprises means 36 enabling the insertion under pressure of gas (pCO 2 and/or CO) into the cathode compartment 33 .
  • gas pCO 2 and/or CO
  • the injection of steam is done via means 35 at the level of anode 32 while the injection of gas CO 2 and/or CO is done via means 36 at the level of cathode 33 .
  • the water is oxidized by releasing electrons while H + ions (in OH o . form) are generated according to a process that is similar to the process described with the help of FIG. 2 .
  • H + ions migrate through the electrolyte 31 , carbon compounds of the CO 2 and/or CO type react at cathode 33 with these H + ions to form compounds of the C x H y O z type (with x>1; y is between 0 and 2x+2 and z is between 0 and 2x) and water at the cathode.
  • C x H y O z compounds synthesized at the cathode depends on many process parameters such as, for example, gas pressure, operating temperature T 1 and the voltage-current pair applied to the cathode as described below:
  • the relative pressure of CO 2 and/or CO is greater than or equal to 1 bar and less than or equal to a burst pressure of the assembly, the latter being greater than or equal to at least 100 bars.
  • relative pressure designates the pressure of insertion with relation to atmospheric pressure.
  • partial pressure will designate either the total pressure of the gas stream in the case where the latter is only constituted of steam or the partial pressure of the steam in the case where the gas stream comprises gases other than steam.
  • T 1 of the device depends on the type of material utilized for membrane 31 ; in any case, this temperature is over 200° C. and is generally under 800° C., or even under 600° C. This operating temperature corresponds to a conduction ensured by W protons.
  • the operating temperature T 1 of the device is also dependent, within the 200 to 800° C. range, according to the nature of the C x H y O z carbon compounds that one wishes to generate.
  • electrodes presenting a large number of triple contact points i.e., points or contact surfaces between an ionic conductor, an electronic conductor and a gas phase.
  • the electrodes considered are preferentially ceramic-metal materials formed by a mixture of ion-conducting ceramic and an electron-conducting metal.
  • all-ceramic electron-conducting electrodes may also be considered instead of a ceramic-metal material.
  • a given electrolyte may be an O 2 ⁇ proton or ion conductor according to the temperature and the pressure of the applied steam.
  • H + ion conducting membranes operating at moderate temperature enables the synthesis of C x HyO z type complex compounds (with x, y and z greater than 1) while the utilization of O 2 ⁇ conducting membranes, operating at a much higher temperature, preferentially generates CO, a product that is stable at high temperature.
  • the objective of studies implemented is to obtain the maximum yield for the production of hydrogen and/or the hydrogenation of CO 2 and/or CO. To do this, most of the current utilized must intervene in the faraday process, i.e., be utilized for the reduction of water and consequently the production of highly reactive hydrogen.
  • the present invention proposes the utilization of proton-conducting electrolyte under steam pressure for the electrolysis of water at high temperature for hydrogen production as well as for electroreduction of CO 2 and/or CO at the cathode.
  • the process comprises the following steps:
  • “highly reactive” hydrogen is produced at the cathode that may generate hydrogen (H 2 ), in the absence of a reducible compound, or C x H y O z type compounds, in the presence of CO 2 and/or CO with x>1; y is between 0 and 2x+2 and z is between 0 and 2x.
  • the proton-conducting membrane is made from a material promoting the insertion of water such as a doped perovskite material of general formula AB 1-x D 2 O 3-x/2 .
  • the materials utilized for the anode and the cathode are preferentially ceramic-metal materials (mixture of metal with the perovskite material utilized for the electrolyte).
  • the membrane is preferably impermeable to O 2 and H 2 gases.
  • the membrane may be of the type: perovskite vacancies, non-stoichiometric perovskites and/or perovskites doped with general formula ABO 3 , of fluorite, pyrochlore A 2 B 2 X 7 , apatite Me 10 (XO 4 ) 6 Y 2 , oxyapatite Me 10 (XO 4 ) 6 O 2 structure, of hydroxylapatite Me 10 (XO 4 ) 6 (OH) 2 structure, silicate structures, aluminosilicates (phyllosilicate or zeolite), silicates grafted with oxyacids or silicates grafted with phosphates.
  • general formula ABO 3 of fluorite, pyrochlore A 2 B 2 X 7 , apatite Me 10 (XO 4 ) 6 Y 2 , oxyapatite Me 10 (XO 4 ) 6 O 2 structure, of hydroxylapatite Me 10 (XO 4 ) 6 (
  • the electrolytes may advantageously be all of the compounds utilized as high temperature or intermediate temperature proton conductors either by virtue of their tunnel or sheet structure and/or by the presence of vacancies capable of inserting protonated species whose molecular size is small.
  • the material enabling the incorporation of protonated species may be impermeable to O 2 and H 2 gases and/or may enable the incorporation of protonated species at a densification level of over 88%, preferably equal at least to 94%.
  • the material enabling the injection of water is an oxygen atom-defective oxide such as an oxygen-defective perovskite acting as a proton conductor.
  • the oxygen atom-defective oxide may present stoichiometric intervals and/or may be doped.
  • non-stoichiometry and/or doping allow the creation of oxygen atom vacancies.
  • the exposure under pressure of a perovskite presenting stoichiometric intervals and/or being doped (and therefore being deficient in oxygen) to steam induces the incorporation of protonated species into the structure.
  • the molecules of water fill the oxygen vacancies and dissociate into 2 hydroxyl groups (or H+ proton on an oxide site) according to the reaction:
  • materials other than non-stoichiometric and/or doped perovskites may be utilized as materials promoting the incorporation of water and its dissociation in the form of protonated species and/or hydroxides.
  • crystallographic structures such as fluorite structures, pyrochlore A 2 B 2 X 7 structures, apatite Me 10 (XO 4 ) 6 Y 2 structures, oxyapatite Me 10 (XO 4 ) 6 O 2 structures, hydroxylapatite Me 10 (XO 4 ) 6 (OH) 2 structures, silicates, aluminosilicates, phyllosilicates, or phosphates may be cited.
  • These structures may possibly be grafted by oxyacid groups.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US12/992,740 2008-05-15 2009-05-15 Process for producing compounds of the cxhyoz type by reduction of carbon dioxide (co2) and/or carbon monoxide (co) Abandoned US20110132770A1 (en)

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FR0853161 2008-05-15
FR0853161A FR2931168B1 (fr) 2008-05-15 2008-05-15 Procede de production de composes du type cxhyoz par reduction de dioxyde de carbone (co2) et/ou de monoxyde de carbone (co)
PCT/FR2009/050909 WO2009150352A2 (fr) 2008-05-15 2009-05-15 Procede de production de composes du type cxhyo2 par reduction de dioxyde de carbone (co2) et/ou de monoxyde de carbone (co)

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EP (1) EP2282983A2 (fr)
JP (1) JP2011521104A (fr)
CN (1) CN102056866A (fr)
BR (1) BRPI0912654A2 (fr)
FR (1) FR2931168B1 (fr)
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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140284220A1 (en) * 2011-10-12 2014-09-25 Areva Method for generating hydrogen and oxygen by steam electrolysis
US10273589B2 (en) * 2013-03-28 2019-04-30 Cuf—Quimicos Industriais S.A. Electrodes/electrolyte assembly, reactor and method for direct amination of hydrocarbons
US10422044B2 (en) 2014-04-02 2019-09-24 Beatrice Sala Electrochemical cell for the electrolysis of liquid water or water vapor, manufacturing process and uses
CN111215111A (zh) * 2020-01-13 2020-06-02 山西大学 一种富含氧空位的二氧化碳电化学还原催化剂及其制备方法和应用
US11001549B1 (en) 2019-12-06 2021-05-11 Saudi Arabian Oil Company Electrochemical reduction of carbon dioxide to upgrade hydrocarbon feedstocks
CN113106485A (zh) * 2021-04-25 2021-07-13 中国华能集团清洁能源技术研究院有限公司 一种电解水双功能电极结构
US11130723B2 (en) 2017-03-14 2021-09-28 Kabushiki Kaisha Toshiba Carbon dioxide electrolytic device
EP3988523A1 (fr) * 2020-10-21 2022-04-27 B. Braun Surgical, S.A. Procédé de production de molécules organiques fonctionnalisées et leurs utilisations
US11420915B2 (en) 2020-06-11 2022-08-23 Saudi Arabian Oil Company Red mud as a catalyst for the isomerization of olefins
US11421330B2 (en) * 2017-03-16 2022-08-23 Battelle Energy Alliance, Llc Methods for carbon dioxide hydrogenation
US11427519B2 (en) 2021-01-04 2022-08-30 Saudi Arabian Oil Company Acid modified red mud as a catalyst for olefin isomerization
US11426708B2 (en) 2020-03-02 2022-08-30 King Abdullah University Of Science And Technology Potassium-promoted red mud as a catalyst for forming hydrocarbons from carbon dioxide
US11495814B2 (en) 2020-06-17 2022-11-08 Saudi Arabian Oil Company Utilizing black powder for electrolytes for flow batteries
US11718522B2 (en) 2021-01-04 2023-08-08 Saudi Arabian Oil Company Black powder catalyst for hydrogen production via bi-reforming
US11724943B2 (en) 2021-01-04 2023-08-15 Saudi Arabian Oil Company Black powder catalyst for hydrogen production via dry reforming
US11814289B2 (en) 2021-01-04 2023-11-14 Saudi Arabian Oil Company Black powder catalyst for hydrogen production via steam reforming
US11820658B2 (en) 2021-01-04 2023-11-21 Saudi Arabian Oil Company Black powder catalyst for hydrogen production via autothermal reforming
US12000056B2 (en) 2020-06-18 2024-06-04 Saudi Arabian Oil Company Tandem electrolysis cell

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WO2012135122A2 (fr) * 2011-03-26 2012-10-04 Honda Motor Co., Ltd. Matériaux et conception pour dispositif électrocatalytique et procédé de production de nanotubes de carbone et de carburants hydrocarbonés de transport
FR2981369B1 (fr) * 2011-10-12 2013-11-15 Areva Procede et systeme de traitement de gaz carbones par hydrogenation electrochimique pour l'obtention d'un compose de type cxhyoz
FR3004179B1 (fr) 2013-04-08 2015-05-01 Commissariat Energie Atomique Procedes d'obtention de gaz combustible a partir d'electrolyse de l'eau (eht) ou de co-electrolyse avec h2o/co2 au sein d'une meme enceinte, reacteur catalytique et systeme associes
JP6292381B2 (ja) * 2014-02-07 2018-03-14 パナソニックＩｐマネジメント株式会社 水蒸気電解水素化装置
JP6610917B2 (ja) * 2014-02-07 2019-11-27 パナソニックＩｐマネジメント株式会社 水蒸気電解水素化装置
DE102015209509A1 (de) * 2015-05-22 2016-11-24 Siemens Aktiengesellschaft Elektrolysesystem zur elektrochemischen Kohlenstoffdioxid-Verwertung mit Protonenspender-Einheit und Reduktionsverfahren

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US4547273A (en) * 1984-06-07 1985-10-15 Energy Conversion Devices, Inc. Mobile atom insertion reaction, mobile atom transmissive membrane for carrying out the reaction, and reactor incorporating the mobile atom transmissive membrane
US20070278092A1 (en) * 2004-03-26 2007-12-06 Irvine John T S Steam Electrolysis
US20100196767A1 (en) * 2007-06-01 2010-08-05 Sala Beatrice Method for optimising the conductivity provided by the displacement of h+ protons and/or oh- ions in a conductive membrane

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Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140284220A1 (en) * 2011-10-12 2014-09-25 Areva Method for generating hydrogen and oxygen by steam electrolysis
US10273589B2 (en) * 2013-03-28 2019-04-30 Cuf—Quimicos Industriais S.A. Electrodes/electrolyte assembly, reactor and method for direct amination of hydrocarbons
US10689767B2 (en) 2013-03-28 2020-06-23 Bondalti Chemicals, S.A. Electrodes/electrolyte assembly, reactor and method for direct amination of hydrocarbons
US10422044B2 (en) 2014-04-02 2019-09-24 Beatrice Sala Electrochemical cell for the electrolysis of liquid water or water vapor, manufacturing process and uses
US11130723B2 (en) 2017-03-14 2021-09-28 Kabushiki Kaisha Toshiba Carbon dioxide electrolytic device
US11421330B2 (en) * 2017-03-16 2022-08-23 Battelle Energy Alliance, Llc Methods for carbon dioxide hydrogenation
US11001549B1 (en) 2019-12-06 2021-05-11 Saudi Arabian Oil Company Electrochemical reduction of carbon dioxide to upgrade hydrocarbon feedstocks
US11339109B2 (en) 2019-12-06 2022-05-24 Saudi Arabian Oil Company Electrochemical reduction of carbon dioxide to upgrade hydrocarbon feedstocks
CN111215111A (zh) * 2020-01-13 2020-06-02 山西大学 一种富含氧空位的二氧化碳电化学还原催化剂及其制备方法和应用
US11426708B2 (en) 2020-03-02 2022-08-30 King Abdullah University Of Science And Technology Potassium-promoted red mud as a catalyst for forming hydrocarbons from carbon dioxide
US11420915B2 (en) 2020-06-11 2022-08-23 Saudi Arabian Oil Company Red mud as a catalyst for the isomerization of olefins
US11495814B2 (en) 2020-06-17 2022-11-08 Saudi Arabian Oil Company Utilizing black powder for electrolytes for flow batteries
US12000056B2 (en) 2020-06-18 2024-06-04 Saudi Arabian Oil Company Tandem electrolysis cell
EP3988523A1 (fr) * 2020-10-21 2022-04-27 B. Braun Surgical, S.A. Procédé de production de molécules organiques fonctionnalisées et leurs utilisations
US11427519B2 (en) 2021-01-04 2022-08-30 Saudi Arabian Oil Company Acid modified red mud as a catalyst for olefin isomerization
US11718522B2 (en) 2021-01-04 2023-08-08 Saudi Arabian Oil Company Black powder catalyst for hydrogen production via bi-reforming
US11724943B2 (en) 2021-01-04 2023-08-15 Saudi Arabian Oil Company Black powder catalyst for hydrogen production via dry reforming
US11814289B2 (en) 2021-01-04 2023-11-14 Saudi Arabian Oil Company Black powder catalyst for hydrogen production via steam reforming
US11820658B2 (en) 2021-01-04 2023-11-21 Saudi Arabian Oil Company Black powder catalyst for hydrogen production via autothermal reforming
CN113106485A (zh) * 2021-04-25 2021-07-13 中国华能集团清洁能源技术研究院有限公司 一种电解水双功能电极结构

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WO2009150352A2 (fr) 2009-12-17
FR2931168B1 (fr) 2010-07-30
RU2493293C2 (ru) 2013-09-20
EP2282983A2 (fr) 2011-02-16
WO2009150352A3 (fr) 2010-02-18
CN102056866A (zh) 2011-05-11
RU2010151465A (ru) 2012-06-20
BRPI0912654A2 (pt) 2016-07-05
JP2011521104A (ja) 2011-07-21
FR2931168A1 (fr) 2009-11-20

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