Classifications

• • 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
  • C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
  • C25B1/46—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in diaphragm cells
• • 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
  • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
  • C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
  • C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
  • C25B11/031—Porous electrodes
  • C25B11/032—Gas diffusion electrodes
• • 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
  • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
  • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
  • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
  • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
  • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
  • C25B11/081—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the element being a noble metal
• • 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
  • C25B13/00—Diaphragms; Spacing elements
• • 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
• • 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
  • C25B15/023—Measuring, analysing or testing during electrolytic production
  • C25B15/025—Measuring, analysing or testing during electrolytic production of electrolyte parameters
  • C25B15/027—Temperature
• • 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
  • C25B15/023—Measuring, analysing or testing during electrolytic production
  • C25B15/025—Measuring, analysing or testing during electrolytic production of electrolyte parameters
  • C25B15/029—Concentration
  • C25B15/031—Concentration pH
• • 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
  • C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
• • 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
  • C25B9/60—Constructional parts of cells
  • C25B9/65—Means for supplying current; Electrode connections; Electric inter-cell connections

Definitions

• the invention relates to a process for the electrolysis of aqueous solutions of alkali metal chlorides by means of gas diffusion electrodes with adherence to particular operating parameters.
• the invention proceeds from electrolysis processes known per se, e.g. for the electrolysis of aqueous alkali metal chloride solutions by means of gas diffusion electrodes which usually comprise an electrically conductive support and a gas diffusion layer having a catalytically active component.
• gas diffusion electrodes which usually comprise an electrically conductive support and a gas diffusion layer having a catalytically active component.
• the arrangement is such that there is a narrow gap through which an electrolyte flows between gas diffusion electrode and ion exchange membrane.
• the gas diffusion electrode hereinafter also referred to as GDE for short, has to meet a number of requirements in order to be able to be used in industrial electrolyzers.
• the catalyst and all other materials used have to be chemically stable to the electrolyte used and the gases supplied to the electrode and also the compounds formed at the electrode, e.g. hydroxide ions or hydrogen, at a temperature of typically up to 90° C.
• a high degree of mechanical stability is likewise required so that the electrodes can be installed and operated in electrolyzers having a size of usually more than 2 m 2 in area (industrial size).
• Further desirable properties are: a high electrical conductivity, a low layer thickness, a high internal surface area and a high electrochemical activity of the electrocatalyst. Suitable hydrophobic and hydrophilic pores and an appropriate pore structure for the conduction of gas and electrolyte are necessary.
• the long-term stability and low production costs are further particular requirements which an industrially usable oxygen-depolarized electrode has to meet.
• WO 2001/57290 A1 describes a cell for chloralkali electrolysis in which the liquid is conveyed from the top downward over a sheet-like porous element, known as a percolator, installed between gas diffusion electrode and ion exchange membrane in a type of free-falling liquid film, referred to as falling film for short, along the gas diffusion electrode (minigap arrangement).
• a percolator a sheet-like porous element
• falling film free-falling liquid film
• a further arrangement which is sometimes also referred to as “zero gap” but would be more precisely formulated as “microgap”, is described in JP 3553775 and U.S. Pat. No. 6,117,286 A1.
• a further layer composed of a porous hydrophilic material which takes up the alkali metal hydroxide solution formed due to its suction force and from which at least part of the alkali can flow away in a downward direction is located between the ion exchange membrane and the GDE.
• the possibility of the alkali metal hydroxide solution flowing away is determined by the installation of the GDE and the cell design.
• An oxygen-depolarized electrode typically consists of a support element, for example a plate of porous metal or a woven fabric made of metal wires, and an electrochemically catalytically active coating.
• the electrochemically active coating is microporous and consists of hydrophilic and hydrophobic constituents.
• the hydrophobic constituents make penetration of electrolyte difficult and thus keep the appropriate pores in the GDE free for transport of oxygen to the catalytically active sites.
• the hydrophilic constituents allow passage of the electrolyte to the catalytically active sites and outward transport of the hydroxide ions from the GDE.
• a fluorine-containing polymer such as polytetrafluoroethylene (PTFE) is generally used as hydrophobic component and additionally serves as polymeric binder for particles of the catalyst.
• PTFE polytetrafluoroethylene
• the silver serves, for example, as hydrophilic component.
• Many compounds have been described as electrochemical catalyst for the reduction of oxygen. However, only platinum and silver have attained practical importance as catalyst for the reduction of oxygen in alkaline solutions.
• Platinum has a very high catalytic activity for the reduction of oxygen. Owing to the high cost of platinum, this is used exclusively in supported form.
• a preferred support material is carbon.
• platinum-based electrodes supported on carbon in long-term operation is unsatisfactory, presumably because platinum also catalyzes the oxidation of the support material.
• carbon promotes the undesirable formation of H 2 O 2 , which likewise brings about oxidation.
• Silver likewise has a high electrocatalytic activity for the reduction of oxygen.
• Silver can be used in carbon-supported form and also as finely divided metallic silver. Although carbon-supported silver catalysts are more durable than the corresponding platinum catalysts, their long-term stability under the conditions in an oxygen-depolarized electrode, in particular during use for chloralkali electrolysis, is also limited.
• the silver is preferably introduced at least partly in the form of silver oxides which are then reduced to metallic silver.
• the reduction generally occurs during the first start-up of the electrolysis cell.
• a change in the arrangement of the crystallites, in particular bridge formation between individual silver particles, also occurs. This leads overall to consolidation of the structure.
• a further central element of the electrolysis cell is the ion exchange membrane.
• the membrane is permeable to cations and water and largely impermeable to anions.
• the ion exchange membranes in electrolysis cells are subject to great stress: they have to be resistant to chlorine on the anode side and strongly alkaline conditions on the cathode side at temperatures of about 90° C.
• Perfluorinated polymers such as PTFE usually withstand these stresses. Ion transport occurs via acidic sulfonate groups and/or carboxylate groups polymerized into these polymers. Carboxylate groups display greater selectivity and the carboxylate-containing polymers have a smaller water absorption and a higher electrical resistance than polymers containing sulfonate groups.
• multilayer membranes having a thicker layer containing sulfonate groups on the anode side and a thinner layer containing carboxylate groups on the cathode side are generally used.
• the membranes are provided with a hydrophilic layer on the cathode side or on both sides.
• the membranes are reinforced by insertion of woven fabrics or nonwovens, and the reinforcement is preferably incorporated in the layer containing sulfonate groups.
• the ion exchange membranes are sensitive to changes in the media surrounding them.
• High osmotic pressure gradients can be built up between anode side and cathode side as a result of different molar concentrations.
• the membrane swells due to increased water absorption.
• the electrolyte concentrations increase, the membrane releases water and shrinks as a result; in the extreme case, precipitation of solids in the membrane or mechanical damage such as cracks in the membrane can occur as a result of withdrawal of water.
• An inhomogeneity of the water and/or ion distribution in the membrane and/or the gas diffusion electrode can lead to local peaks in electricity transport and mass transfer on renewed start-up and consequently to damage to the membrane or the gas diffusion electrode.
• U.S. Pat. No. 4,578,159 A1 states that damage to membrane and electrode is avoided in an electrolysis process using a “zero gap” arrangement by flushing of the cathode space with 35% strength sodium hydroxide solution before start-up of the cell or by starting the cell at a low current density and gradually increasing the current density. This procedures reduces the risk of damage to membrane and gas diffusion electrode during start-up, but offers no protection against damage during shutdown and the downtime.
• One measure known from conventional membrane electrolysis is maintenance of a polarization voltage, i.e. the voltage is not regulated down to zero on ending of the electrolysis but instead a residual voltage is maintained so that a residual current flows in the usual electrolysis direction, so that a constant small current density results and as a result an electrolysis occurs to a small extent. If the electrolysis is to be shut down, cooling of the electrolyte is necessary, as a result of which the potentials change. This measure alone is therefore not sufficient to prevent damage to the electrode during start-up and shutdown when using gas diffusion electrodes.
• the alkali metal hydroxide is preferably sodium hydroxide or potassium hydroxide, particularly preferably sodium hydroxide.
• the gas diffusion electrode is supplied with oxygen gas on its side facing away from the catholyte during operation.
• the oxygen gas stream to the gas diffusion electrode is preferably maintained during shutdown of the electrolysis according to the new process.
• the purity of the oxygen corresponds to the concentrations and purity requirements customary in electrolysis using a gas diffusion electrode; oxygen having a content of more than 98.5% by volume is preferably used.
• the temperature of the catholyte fed in is regulated during operation so that a temperature of 70-95° C., preferably 75-90° C., is established in the output from the cathode space.
• a temperature difference between anolyte output and catholyte input is preferably set to less than 20° C. during operation and during shutdown. Such a small temperature difference avoids damage to the ion exchange membrane.
• a brine having a content of NaCl of from 180 g/l (3.07 mol/l) to 330 g/l (5.64 mol/l) is fed into the anode space in a preferred embodiment.
• the anode space is freed of chlorine gas present and the content of dissolved/dispersed chlorine is reduced.
• a current density of from greater than zero to 20 A/m 2 is preferably maintained.
• the electrolysis is operated until the anolyte is Cl 2 -free, i.e. the content of chlorine having the oxidation state zero is from >0 to less than 10 mg/l.
• the measurement of the absence of chlorine in the anolyte is, in particular, carried out by means of redox titration such as iodometry or by testing of the anolyte by means of iodine-starch paper.
• the maintenance of the brine pH in the range from 2 to 12, preferably from 6 to 9, during step a) is required in order to avoid any chlorine evolution at a lower pH.
• the temperature of the anolyte in steps a) and b) is preferably at least 65° C., particularly preferably at least 70° C.
• the anolyte is cooled in step d) to a temperature below 70° C. with simultaneous maintenance of an electrolysis voltage of from 0.1 to 1.4 V. This is a further difference from the prior art—cooling is carried out there without maintenance of the electrolysis voltage.
• the switching off of the electrolysis voltage in step e) is carried out at a temperature of the electrolytes of ⁇ 55° C., preferably at a temperature of ⁇ 50° C.
• the cathode gap (minigap) is subsequently emptied in step f) (e.g. by switching off the pump for the catholyte feed).
• step f e.g. by switching off the pump for the catholyte feed.
• the emptying of the anode space in step g) is carried out by draining the anolyte and, in particular, subsequent flushing h) of the anode space with alkali metal chloride solution having a maximum concentration of 4 mol/ 1 or with deionized water.
• the cathode gap (minigap) is flushed with dilute sodium hydroxide solution or deionized water to remove chloride residues and empty the cathodic minigap.
• the cathode gap here is flushed again in order to remove chloride after the anode space has been emptied. This avoids, for example, corrosion on nickel connecting flanges of the cell by excessively high chloride values in the alkali remaining in the cathode space.
• residual emptying of the anode space can particularly preferably then be carried out.
• the emptying of the anode space takes up to 150 minutes, depending on cell construction at an industrial construction size.
• the pH of the brine is not taken into consideration in the prior art, while according to the invention this is optimally from 2 to 12.
• the gas diffusion electrode is efficiently protected by the process of the invention.
• the cell can also be cooled to below 70° C. without chlorine being evolved on the anode side as a result of the potentiostatic operation. This is important from safety aspects if the electrolysis elements are to be opened later for maintenance work or repair.
• the electrolysis voltage is regulated down.
• the voltage is regulated down to a value of from 0.1 to 1.4 V.
• the chlorine content in the anode space is lowered to ⁇ 10 mg/l, preferably less than 1 mg/l.
• the pH of the anolyte in the output from the electrolysis cell is from 2 to 12, preferably from 6 to 9.
• the chlorine content is the total content of dissolved chlorine in the oxidation state 0 and above.
• Removal of the remaining chlorine from the anode space is preferably effected by chlorine-free anolyte being fed in with simultaneous discharge of chlorine-containing anolyte, or by pumping of the anolyte in the anode circuit with simultaneous removal and discharge of chlorine gas.
• the voltage is set during flushing free of Cl2 so that a current density of from 0.01 to 20 A/m 2 , preferably from 10 to 18 A/m 2 , is established.
• the electrolysis is not operated below a temperature of 70° C., since otherwise chlorine evolution recommences.
• the cooling of the electrolysis can be carried out according to the process of the invention when the electrolysis voltage below a temperature of 70° C. is not more than 1.4 V, with the pH of the brine being in the range from 2 to 12. In this state, the electrolysis can be suspended for many hours without the gas diffusion electrode being damaged. Relative to the prior art, the electrolysis voltage continues to be applied.
• the electrolysis cell with the moist membrane can be kept ready over a relatively long period of time in the built-in state for a quick start-up without the performance capability of the electrolysis cell being impaired.
• the concentration of the dilute alkali metal chloride solution used for flushing or wetting is 1-4.8 mol/l.
• the flushing solution can be drained off again immediately after complete filling of the anode space or reside in the anode space for up to 200 minutes and then be drained off.
• the concentration of the alkali metal hydroxide solution used for flushing or wetting is from 0.1 to 10 mol/l, preferably from 1 to 4 mol/l.
• the temperature of the brine or the alkali metal hydroxide solution can be in the range from 10 to 80° C., but is preferably from 15 to 40° C.
• the flushing of the minigap cathode shells can be carried out for a period of from 0.1 to 10 minutes.
• the invention also provides a process for start-up, in particular for restarting after the new process for shutdown.
• the restarting of the electrolysis is, in particular, carried out as follows:
• Anolyte is, as per step j), introduced into the anode space of the cell and, in particular, heated to at least 50° C. in a circuit with heat exchanger,
• Catholyte is, for step k), heated to a temperature of at least 50° C. outside the cell, e.g. in a circuit with storage vessel and heat exchanger.
• the cathode gap (minigap) is filled as per step 1 ) by the preheated alkali metal hydroxide solution having a temperature of at least 50° C. being introduced into the gap.
• an electrolysis voltage of at least 0.4 V is preferably applied in step m), in particular within from 0.01 to 10 minutes, so that a current density of at least 0.2 A/m 2 is established.
• Anolyte and catholyte are subsequently heated to a temperature of at least 70° C. as per step n) and the current density is then preferably increased.
• the increase in the current density to the production current density in step q) is particularly preferably effected at a rate of from 0.018 kA/(m 2 *min) to 0.4 kA/(m 2 *min) until the current density at the electrolysis element is at least 2 kA/m 2 .
• the electrolysis cell which has been shut down according to the above new process is restarted according to the above-described new process.
• the electrolysis cell can go through many start-up and running-down cycles without the performance of the cell being impaired.
• the gas diffusion electrode used in the examples was produced as described in EP 1728896 B1, as follows: a powder mixture consisting of 7% by weight of PTFE powder, 88% by weight of silver(I) oxide and 5% by weight of silver powder was applied to a gauze made of nickel wires and pressed to give an oxygen-depolarized electrode.
• the electrode was installed in an electrolysis unit having an area of 100 cm 2 with a DuPONT type N982 ion exchange membrane (manufactured by Chemours) and a spacing between gas diffusion electrode and ion exchange membrane of 3 mm.
• the electrolysis unit has, in the assembled state, an anode space having an anolyte inlet and outlet and an anode consisting of titanium expanded metal which was coated with a commercial DSA coating for chlorine production from Denora, consisting of a mixed oxide of ruthenium oxide/iridium oxide, and a cathode space having the gas diffusion electrode as cathode and having a gas space for the oxygen and oxygen inlets and outlets, a liquid outlet and an ion exchange membrane, which are arranged between anode space and cathode space.
• a commercial DSA coating for chlorine production from Denora consisting of a mixed oxide of ruthenium oxide/iridium oxide
• a cathode space having the gas diffusion electrode as cathode and having a gas space for the oxygen and oxygen inlets and outlets, a liquid outlet and an ion exchange membrane, which are arranged between anode space and cathode space.
• the electrolysis cell was operated at a brine concentration of about 210 g/l (3.58 mol/l) of NaCl and a sodium hydroxide concentration of about 31% by weight (10.4 mol/l) at electrolyte temperatures of about 85° C.
• the cell voltage was corrected to 32% by weight (10.79 mol/l) of sodium hydroxide and 90° C. by customary standard methods.
• the electrolytes were each introduced into the cell from below and taken off again from the top of the cell.
• Oxygen was fed to the gas space of the cathode.
• An oxygen having a purity of more than 99.5% by volume of oxygen was used here.
• the oxygen was humidified with water at room temperature before being introduced into the gas space of the cathode half shell.
• the amount of oxygen was regulated so that a 1.5-fold stoichiometric excess over the amount of oxygen required based on the current strength set was always introduced.
• the oxygen is fed from the top into the gas space and discharged at the bottom.
• the electrolysis unit had a gap of about 3 mm between oxygen-depolarized electrode and ion exchange membrane. This gap was filled with a porous PTFE woven fabric as percolator and spacer.
• the production current density was 6 kA/m 2 .
• the anolyte circuit was, according to the invention, started up and the anode space was filled with an anolyte having a concentration of about 210 g of NaCl/l (3.58 mol/l). While the anode circuit was maintained and the anolyte was conveyed through the cell, the anolyte was heated to 50° C. by means of a heat exchanger present in the anode circuit.
• the sodium hydroxide solution having a temperature of 50° C. was fed into the cell and, after filling of the cathode gap within 30 seconds, an electrolysis voltage of 1.08 V was applied. This resulted in a current density of 10 mA/cm 2 being established.
• the pH of the outflowing anolyte was 8.
• the electrolyte was heated from 50° C. to 70° C. within 1 hour. After the temperature of the outflowing anolyte and catholyte of 70° C. had been attained, the electrolysis voltage was increased, with the electrolysis voltage being increased such that the current density was raised every 2 minutes by 50 mA/cm 2 up to a current density of 600 mA/cm 2 .
• concentrations were regulated after start-up so that the concentration of the outflowing brine was about 210 g/l (3.59 mol/l) and that of the sodium hydroxide solution was about 31.5% by weight (10.6 mol/l).
• the cell was operated for at least 24 hours under these conditions.
• the current density was reduced to 1.5 mA/cm 2 .
• the main rectifier was disconnected and the polarization rectifier was switched in.
• the polarization rectifier then takes over maintenance of a current density of 1.5 mA/cm 2 .
• the operation at the low current density was maintained for 1.5 hours.
• the anolyte is chlorine-free.
• This process is carried out in industrial electrolyzers for safety reasons.
• One of the reasons is that chlorine or chlorine compounds such as hypochlorite do not diffuse from the anolyte through the ion exchange membrane into the catholyte and lead there to corrosion of cell components or the gas diffusion electrode.
• the phase of chlorine-free flushing takes about 1.5 hours in industrial electrolyzers.
• Electrolyte circuits remained in operation with the same volume flows as in electrolysis operation at 600 mA/cm 2 .
• the O 2 supply was likewise maintained.
• the temperature of the anolyte and of the catholyte was reduced from 85° C. to 70° C.
• the cell voltage during this phase was about 1.16 V and the pH of the outflowing anolyte from the cell was pH 8.2.
• the polarization rectifier is disconnected and the catholyte is immediately drained from the cathode space. This occurs over a time of about 30 seconds. After emptying of the cathode space, the anode space is drained within 1 hour.
• the anode space is filled with deionized water from below up to a height of max. 50% of the cell height and immediately drained off again.
• the cathode gap was likewise flushed by renewed switching-on of the catholyte pump and feeding of catholyte into the cathode space.
• the catholyte pump was switched on for about 10 seconds.
• the catholyte gap ran empty within 15 seconds.
• the cell was then allowed to stand for 10 hours.
• the cell voltage remained unchanged and damage to the gas diffusion electrode and further components did not occur.
• the cell voltage increased by 30 mV, and damage to the gas diffusion electrode occurred.

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• 2018
  • 2018-12-18 EP EP18213272.0A patent/EP3670706B1/de active Active
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