EP3317435B1 - Reduktionsverfahren und elektrolysesystem zur elektrochemischen kohlenstoffdioxid-verwertung - Google Patents

Reduktionsverfahren und elektrolysesystem zur elektrochemischen kohlenstoffdioxid-verwertung Download PDF

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Publication number
EP3317435B1
EP3317435B1 EP16726551.1A EP16726551A EP3317435B1 EP 3317435 B1 EP3317435 B1 EP 3317435B1 EP 16726551 A EP16726551 A EP 16726551A EP 3317435 B1 EP3317435 B1 EP 3317435B1
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EP
European Patent Office
Prior art keywords
electrolyte
reservoirs
carbon dioxide
electrolysis system
reservoir
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.)
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Application number
EP16726551.1A
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German (de)
English (en)
French (fr)
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EP3317435A1 (de
Inventor
Philippe Jeanty
Maximilian Fleischer
Ralf Krause
Erhard Magori
Nayra Sofia ROMERO CUÉLLAR
Bernhard Schmid
Günter Schmid
Kerstin Wiesner-Fleischer
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Siemens AG
Siemens Corp
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Siemens AG
Siemens Corp
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Priority to PL16726551T priority Critical patent/PL3317435T3/pl
Publication of EP3317435A1 publication Critical patent/EP3317435A1/de
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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
    • C25B15/00—Operating or servicing cells
    • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
    • 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
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/20—Processes
    • C25B3/25—Reduction
    • 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
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof

Definitions

  • the present invention relates to a method and an electrolysis system for electrochemical carbon dioxide utilization. Carbon dioxide is introduced into an electrolytic cell and reduced at a cathode.
  • Electrolysis systems for the electrochemical reduction of carbon dioxide are known, for example from the DE 10 2013 226357 A1 or the US 2012/228148 A1 ,
  • a typical simplified structure of an electrolysis system comprises an electrolytic cell having an anolyte and a catholyte circuit.
  • the circuits are separated by an ion exchange membrane in the electrolysis cell.
  • the respective electrolyte is kept in reservoirs and purified there.
  • the pH value and the ion concentration in the individual solutions change after prolonged operation of the electrolysis.
  • the membrane makes the compensation even more difficult.
  • a 0.5M KHCO3 solution is used as the anolyte and catholyte, the cell voltage rises sharply after a few hours since the cations have migrated from the anolyte space into the catholyte space to the electrode due to the applied electrical voltage.
  • the osmotic pressure is initially balanced or even counteracts after some time, the electrical attraction of the cathode is stronger and cation migration is unidirectional.
  • the equalizing line for the replacement of the liquid electrolyte, it is expedient to connect the equalizing line as far as possible to both electrolyte reservoirs, for example in the lower half of the height of the respective reservoir, in particular in the lower quarter.
  • a pump is present in the pressure compensation connection. This ensures a forced electrolyte exchange.
  • the input signals from level sensors are preferably used for both reservoirs.
  • the two reservoirs can be realized as separate containers, wherein the pressure equalization connection is designed, for example, as a pipe between the containers.
  • the two reservoirs can also be designed together as a single container with a partition wall for subdivision into the two reservoirs, wherein the partition wall has an opening as a pressure equalization connection.
  • the opening is located conveniently in the lower part of the reservoirs to allow replacement of the liquid electrolyte even at low liquid level.
  • the electrolysis system expediently comprises pumps in the first and third connecting lines, which convey the electrolyte to the anode compartment and the cathode compartment. Furthermore, this includes Electrolysis system expedient a supply line for supplying the carbon dioxide.
  • the electrolysis system comprises pressure regulating means for at least one of the reservoirs.
  • the supply line for supplying the carbon dioxide may have a pressure relief valve. If this opens, the carbon dioxide flowing through can then be mixed with the product gas from the first product gas line and conducted together to form an analytic and / or a product gas reservoir.
  • the product gas lines are combined in a pressure relief valve. By a suitable choice of the pressure relief valve thereby an equal pressure in the gas phase is ensured in the reservoirs.
  • the electrolysis system comprises means for introducing inert gas, in particular nitrogen, into the reservoirs.
  • inert gas in particular nitrogen
  • the inlets at the reservoirs are expediently arranged in the lower region of the respective reservoir and the reservoirs comprise in the lower region a layer of glass frit which is permeable to the inert gas.
  • the cathode of the electrolysis system comprises silver, copper, copper oxide, titanium dioxide or another metal oxide semiconductor material.
  • the cathode can also be configured as a photocathode, with which a photoelectrochemical reduction process for the utilization of carbon dioxide could be operated, a so-called photoassisted CO 2 -electrolysis.
  • this system can also work purely photocatalytically.
  • the electrolysis system preferably comprises a platinum anode. KHCO3, K2SO4 and K3PO4 are preferably used as electrolyte salts in different concentrations.
  • potassium iodide KI potassium bromide KBr, potassium chloride KCl, sodium bicarbonate NaHCO 3 , sodium sulfate Na 2 SO 4 can be used.
  • other sulfates, phosphates, iodides or bromides can be used to increase the conductivity in the electrolyte.
  • a surface protective layer it is meant that a relatively thin layer as compared to the total electrode thickness separates the cathode from the cathode space.
  • the surface protection layer may for this purpose comprise a metal, a semiconductor or an organic material.
  • Particularly preferred is a titanium dioxide protective layer. The protective effect is aimed predominantly at the fact that the electrode is not attacked by the electrolyte or reactants, products or catalysts dissolved in the electrolyte and their dissociated ions, and, for example, ions are released from the electrode.
  • a suitable surface protective layer is of great importance for the longevity and functional stability of the electrode in the process.
  • the overvoltages of hydrogen gas H 2 or carbon monoxide gas CO can be influenced in aqueous electrolytes or water-containing electrolyte systems. The consequence would be, on the one hand, a drop in the current density and correspondingly a very low system efficiency for the carbon dioxide conversion and, on the other hand, the mechanical destruction of the electrode.
  • the electrolysis system 100 shown schematically initially has as a central element an electrolytic cell 1, which is shown here in a two-chamber structure.
  • An anode 4 is arranged in an anode space 2, a cathode 5 in a cathode space 3.
  • Anode space 2 and cathode space 3 are separated by a membrane 21.
  • the membrane 21 may be an ion-conducting membrane 21, for example an anion-conducting membrane 21 or a cation-conducting membrane 21.
  • the membrane 21 may be a porous layer or a diaphragm.
  • membrane 21 may also be understood to mean a spatial ion-conducting separator which separates electrolytes into anode and cathode chambers 2, 3. For introducing the carbon dioxide CO 2 into the electrolysis cell 1, this comprises a gas diffusion electrode.
  • Anode 4 and cathode 5 are each electrically connected to a power supply.
  • the anode compartment 2 and the cathode compartment 3 of the electrolysis cell 1 shown are each equipped with an electrolyte inlet and electrolyte outlet, via which the electrolyte and electrolysis by-products, eg oxygen gas O 2 from the anode compartment 2 and cathode compartment, 3 can flow in and out.
  • Anode space 2 and cathode space 3 are integrated via a first to fourth connection line (9 ... 12) in an electrolyte circuit.
  • the electrolyte flow directions are in both Circuits represented by arrows.
  • a first and a second reservoir 6, 7 are integrated into the electrolyte circuit, in which the electrolyte is kept.
  • the electrolyte circuit is formed in contrast to known carbon dioxide electrolysis systems as cross-flow.
  • a first of the connecting lines 9 carries electrolyte and optionally dissolved therein or mixed with educts and products from the first reservoir 6, conveyed by a pump 8a, to the anode chamber 2 and its electrolyte inlet.
  • a second connecting line 10 leads the electrolyte with admixed substances to the second reservoir 7.
  • the electrolyte is therefore not returned to the original reservoir 6.
  • Electrolyte from the second reservoir 7 in turn is conveyed through a third connecting line 11 by means of a pump 8b to the cathode chamber 3.
  • Electrolyte from the cathode chamber 3 is guided via a fourth connecting line 12 to the first reservoir 6. In this way, an entangled cycle for the electrolyte results, in which a given amount of electrolyte reaches and passes through both reservoirs and anode and cathode compartments 2, 3 over time and at least in part.
  • the reservoirs 6, 7 are connected by means of a compensation tube 13.
  • the outlets to the equalization tube 13 in the reservoirs 6, 7 are expediently mounted in the lower part of the reservoir, to allow an exchange of liquid even at low level of the liquid. It is ensured by the compensation tube 13 that none of the reservoirs 6, 7 can idle and that the same height of the electrolyte level is present in both.
  • Fig. 2 shows a more detailed view of the two reservoirs 6, 7.
  • the resulting products such as O2 at the anode 4 and CO at the Cathode 5 transported separately and separated in the reservoirs 6, 7 from the liquid 201.
  • the product gas separation takes place by means of a gas scrubber.
  • nitrogen N2 is introduced, dispersed over a layer 202 of glass frit.
  • This inert gas drives the dissolved gases O2, CO and CO2 out of the electrolyte 201.
  • the electrolyte 201 is typically not gas-free, a certain amount of a certain gas is dissolved in it.
  • CO2 or other inert gases can be used instead of N2. Diluted with the inert gas, the products are removed from the circulation and then analyzed and purified.
  • first product gas line 14 From the first reservoir 6 performs a first product gas line 14. This connected via a first pressure relief valve with a supply line 16 for carbon dioxide, which transports the carbon dioxide to the electrolytic cell 1. If necessary, carbon dioxide, which is not released into the electrolytic cell 1 when the pressure is exceeded, as well as product gas together with the inert gas from the first reservoir 6 of an analytic and an in Fig. 1 not shown product memory is passed. For the calculation of the yield, the amount of the introduced carbon dioxide can be used.
  • a second product gas line 15 from the second reservoir 7 is guided with the common line of first product gas line 14 and carbon dioxide feed line 16 to a second pressure relief valve 18.
  • This controlled combination of the product gas lines 14, 15 from the reservoirs 6, 7 ensures that the pressure in both reservoirs 6, 7 is the same and thus the liquid levels are not displaced. Furthermore, it is advantageous if a regulated pressure control monitors the differential pressure at the GDE, so that it is not subjected to excessive mechanical stress.
  • the second pressure relief valve 18 is set to ensure that no product gas of the anode 4 enters the analytics.
  • Fig. 2 also shows the equalizing tube 13 between the two reservoirs 6, 7.
  • the filling of the reservoirs 6, 7 changes in the described entangled cycle, if not both pumping currents are exactly equal. Although this is achievable via a level measurement and regulation of the pump power, it is complicated and prone to error.
  • FIG. 3 Another embodiment for the two reservoirs 6, 7 is in FIG. 3 shown.
  • the reservoirs 6, 7 configured as a common container 31.
  • the container 31 comprises a partition wall 32, which has an interruption or an opening 33.
  • the opening 33 is expediently located in the lower part of the container 31 in order to enable a constant exchange of the electrolyte 201 between the reservoirs 6, 7.
  • the result of the shared container is largely the same functionality as in the case of the locally separated reservoirs 6, 7.
  • FIG. 4 Another alternative embodiment is in FIG. 4 shown.
  • This embodiment is based on separate reservoirs 6, 7 as the first embodiment.
  • no pressure compensation for the gas phase provided. Different pressure in the two reservoirs 6, 7 can therefore ensure a different electrolyte level and this is not compensated by the equalizing tube, so the simple connection of the two reservoirs 6, 7.
  • the compensation is performed by a pump 42 in this example.
  • the control of the pump is effected by a control electronics, not shown in Figure 4.
  • As input variables for the control sensor signals of two level sensors 41 are used, which detect the level of the electrolyte in both reservoirs 6, 7.
  • a shift in the electrolyte level is compensated by different flow rates of electrolyte to the anode compartment 2 and cathode compartment 3.

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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)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
EP16726551.1A 2015-07-03 2016-05-31 Reduktionsverfahren und elektrolysesystem zur elektrochemischen kohlenstoffdioxid-verwertung Active EP3317435B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL16726551T PL3317435T3 (pl) 2015-07-03 2016-05-31 Sposób redukcji i system elektrolizy do elektrochemicznego stosowania dwutlenku węgla

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102015212503.3A DE102015212503A1 (de) 2015-07-03 2015-07-03 Reduktionsverfahren und Elektrolysesystem zur elektrochemischen Kohlenstoffdioxid-Verwertung
PCT/EP2016/062253 WO2017005411A1 (de) 2015-07-03 2016-05-31 Reduktionsverfahren und elektrolysesystem zur elektrochemischen kohlenstoffdioxid-verwertung

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EP3317435A1 EP3317435A1 (de) 2018-05-09
EP3317435B1 true EP3317435B1 (de) 2019-07-03

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Country Link
US (1) US10760170B2 (pl)
EP (1) EP3317435B1 (pl)
CN (1) CN107849713B (pl)
AU (1) AU2016290263B2 (pl)
DE (1) DE102015212503A1 (pl)
DK (1) DK3317435T3 (pl)
ES (1) ES2748807T3 (pl)
PL (1) PL3317435T3 (pl)
SA (1) SA518390682B1 (pl)
WO (1) WO2017005411A1 (pl)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4004259B1 (de) 2019-09-05 2022-10-19 thyssenkrupp nucera AG & Co. KGaA Kreuzflusswasserelektrolyse

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DE102015212503A1 (de) 2015-07-03 2017-01-05 Siemens Aktiengesellschaft Reduktionsverfahren und Elektrolysesystem zur elektrochemischen Kohlenstoffdioxid-Verwertung
DE102017216710A1 (de) * 2017-09-21 2019-03-21 Siemens Aktiengesellschaft Elektrolyseuranordnung
EP3489389A1 (de) * 2017-11-24 2019-05-29 Siemens Aktiengesellschaft Elektrolyseeinheit und elektrolyseur
US11105006B2 (en) * 2018-03-22 2021-08-31 Sekisui Chemical Co., Ltd. Carbon dioxide reduction apparatus and method of producing organic compound
DE102018210303A1 (de) * 2018-06-25 2020-01-02 Siemens Aktiengesellschaft Elektrochemische Niedertemperatur Reverse-Watergas-Shift Reaktion
US11390955B2 (en) * 2019-08-07 2022-07-19 Sekisui Chemical Co., Ltd. Electrochemical cell, electrochemical system, and method of producing carbonate compound
CN110344071B (zh) * 2019-08-14 2020-11-17 碳能科技（北京）有限公司 电还原co2装置和方法
CN114405438B (zh) * 2022-03-01 2022-11-11 中山大学 一种光电催化反应系统
JP7664879B2 (ja) * 2022-03-22 2025-04-18 株式会社東芝 電解装置および電解装置の駆動方法
CN114689671B (zh) * 2022-03-29 2023-05-16 嘉庚创新实验室 电化学反应设备
DE102023201802A1 (de) 2023-02-28 2024-08-29 Siemens Energy Global GmbH & Co. KG Anordnung für die Gas-Flüssigkeits-Trennung und deren Verwendung
DE102023209118A1 (de) 2023-09-20 2025-03-20 Robert Bosch Gesellschaft mit beschränkter Haftung Die Erfindung betrifft ein Elektrolysesystem, wie es zur elektrolytischen Spaltung von Wasser in Wasserstoff und Sauerstoff mit Hilfe elektrischer Energie verwendet werden kann
DE102024100840A1 (de) * 2024-01-12 2025-07-17 Deutsches Zentrum für Luft- und Raumfahrt e.V. Alkalische Elektrolyseeinrichtung
DE102024210430A1 (de) 2024-10-30 2026-04-30 Robert Bosch Gesellschaft mit beschränkter Haftung Verfahren zum Betreiben einer elektrochemischen Anlage sowie elektrochemische Anlage

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DE102013226357A1 (de) 2013-12-18 2015-06-18 Siemens Aktiengesellschaft Pulsierende Elektrolytzufuhr in den Reaktionsraum einer Elektrolysezelle mit gasentwickelnden Elektroden
WO2015143560A1 (en) * 2014-03-25 2015-10-01 Colin Oloman Process for the conversion of carbon dioxide to formic acid
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Publication number Publication date
AU2016290263B2 (en) 2018-08-30
DE102015212503A1 (de) 2017-01-05
CN107849713B (zh) 2019-08-30
EP3317435A1 (de) 2018-05-09
US10760170B2 (en) 2020-09-01
US20180179649A1 (en) 2018-06-28
WO2017005411A1 (de) 2017-01-12
CN107849713A (zh) 2018-03-27
SA518390682B1 (ar) 2021-09-08
DK3317435T3 (da) 2019-09-23
AU2016290263A1 (en) 2018-01-04
ES2748807T3 (es) 2020-03-18
PL3317435T3 (pl) 2020-03-31

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