DE102014002450A1 - Process for the oxidative degradation of nitrogenous compounds in waste water - Google Patents

Process for the oxidative degradation of nitrogenous compounds in waste water Download PDF

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Publication number
DE102014002450A1
DE102014002450A1 DE102014002450.4A DE102014002450A DE102014002450A1 DE 102014002450 A1 DE102014002450 A1 DE 102014002450A1 DE 102014002450 A DE102014002450 A DE 102014002450A DE 102014002450 A1 DE102014002450 A1 DE 102014002450A1
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Prior art keywords
anode
nitrogen
current density
compounds
cathode
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Withdrawn
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DE102014002450.4A
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German (de)
Inventor
Barbara Behrendt-Fryda
Matthias Fryda
Linda Heesch
Thorsten Matthée
Jens Saalfrank
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Condias GmbH
Areva GmbH
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Condias GmbH
Areva GmbH
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Priority to DE102014002450.4A priority Critical patent/DE102014002450A1/en
Publication of DE102014002450A1 publication Critical patent/DE102014002450A1/en
Withdrawn legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4672Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • C02F2001/46133Electrodes characterised by the material
    • C02F2001/46138Electrodes comprising a substrate and a coating
    • C02F2001/46147Diamond coating
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2201/00Apparatus for treatment of water, waste water or sewage
    • C02F2201/46Apparatus for electrochemical processes
    • C02F2201/461Electrolysis apparatus
    • C02F2201/46105Details relating to the electrolytic devices
    • C02F2201/46115Electrolytic cell with membranes or diaphragms
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2201/00Apparatus for treatment of water, waste water or sewage
    • C02F2201/46Apparatus for electrochemical processes
    • C02F2201/461Electrolysis apparatus
    • C02F2201/46105Details relating to the electrolytic devices
    • C02F2201/4612Controlling or monitoring
    • C02F2201/46125Electrical variables
    • C02F2201/4614Current
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/44Time
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/02Specific form of oxidant
    • C02F2305/023Reactive oxygen species, singlet oxygen, OH radical

Abstract

In a method for the oxidative degradation of nitrogen-containing compounds in wastewater by means of an electrochemical treatment using a diamond electrode as the anode (A) and a cathode (K) as the counter electrode, the destruction of the nitrogen-containing compounds and a reduction of the total nitrogen content in one achieve common method in that in a first stage of the method at the anode (A), a first current density is set to oxidize the nitrogen-containing compounds and then with a second current density, which is less than the first current density, the total dissolved nitrogen content Release of molecular nitrogen is reduced.

Description

  • The invention relates to a process for the oxidative degradation of nitrogen-containing compounds in wastewaters by means of an electrochemical treatment using a diamond electrode as anode and a cathode as counterelectrode.
  • It has been known for some time to perform the treatment of wastewater electrochemically with a diamond electrode as the anode. Diamond electrodes consist of a metallic or non-metallic conductive support on which a layer of diamond crystals is deposited. The diamond layer formed in this way is made conductive by being doped with suitable elements, preferably with boron. The diamond layer is applied to the electrode carrier usually by the CVD (Chemical Vapor Deposition) method and is known to the person skilled in the art by numerous publications (cf. eg US 5,399,247 ).
  • Diamond electrodes have the advantage of allowing a high overpotential, which generates in situ strong oxidants such as ozone, hydrogen peroxide and OH radicals from the wastewater. It is therefore possible with diamond electrodes to produce otherwise difficult to obtain oxidation products. In wastewater treatment, the oxidation by means of the diamond electrodes is operated until the organic components have been completely or almost completely mineralized, ie converted into non-critical compounds (eg CO 2 and water). Such treated water can be reused as service water or discharged as clean wastewater into public waters.
  • In some applications, an amine-containing wastewater is present. For example, treated water is used for the treatment of the water-steam cycle of nuclear power plants with alkalizing, which is present after treatment as waste water with a high amine content. The alkalizing agents used are, for example, ethanolamine, morpholine, dimethylamine and methoxypropylamine.
  • If such an amine-containing wastewater is treated electrochemically, although the respective toxic alkalizing agent can be destroyed, ammonium and nitrates are formed as treatment products which remain dissolved in the wastewater, at least predominantly. Such wastewater must not be disposed of in soils or waters because of the high nitrogen content. It is therefore usually fed to a biological denitrification in a clarifier. This denitrification is technically problematic in highly nitrogenous wastewater and also tedious.
  • The present invention is therefore based on the object to replace the previous biological denitrification by a simpler and better controlled process.
  • To solve this problem, the method of the type mentioned is according to the invention characterized in that in a first stage of the anode, a first current density is set to oxidize the nitrogen-containing compounds and then with a second current density, which is less than the first current density , the dissolved total nitrogen content is reduced by release of molecular nitrogen.
  • The inventive method is based on a plurality of essential principles that have been determined in part by intensive involvement of the inventors with the diamond electrodes.
  • Unlike other electrodes that are used as anodes for the oxidative electrochemical treatment of wastewater, such as platinum electrodes, diamond electrodes, which are operated with an overvoltage of more than 2 V (preferably with 2.4 V), arise from the water OH radicals. Diamond electrodes are thus not selective as a function of the overvoltage, but produce OH radicals independently of the operating voltage. The formation of hydrogen peroxide ozone results from reactions of the short-lived OH radicals, which form an ozone molecule at a high concentration of three OH radicals and form hydrogen peroxide at a lower concentration of two OH radicals. If the concentration of hydroxyl radicals is insufficient for the formation of said secondary products, they directly oxidize constituents of the water.
  • Thus, it is possible to control the type of treatment of the waste water by generating a high or a lower density of OH radicals on the surface of the anode. This control can be done by an appropriate power control. In addition, the shape of the surface of the anode body - and thus the diamond layer - can be exploited for the generation of defined current densities.
  • The oxidation of the contaminants by the OH radicals themselves requires that the corresponding contamination molecules reach the surface of the anode, since the resulting OH radicals have an extremely short life. The oxidation by OH radicals is therefore diffusion-limited. In contrast, a high density of OH radicals leads to the formation of ozone (O 3 ), which is soluble in water. The volume of water in the anode compartment can therefore have a high content of dissolved ozone. It turned out that that Oxidation potential of ozone (2.1 V) is sufficient to destroy the alkalizers by oxidation. Since the ozone is present in solution in all of the water in the anode compartment, effective destruction of the alkalizing agents is effected when the ozone electrode generates much ozone which is suitably dissolved.
  • For the solution of the ozone, it must be ensured that a suitable flow guidance for the water is observed. For example, the formation of turbulence on the anode surface results in the formation of only small O 3 bubbles which, due to their relatively large surface area by volume, result in an improved solution of the ozone in the water from the formation of large bubbles. The solubility of ozone is also dependent on the temperature of the water and decreases with increasing temperature.
  • The adjustment of the current density at the surface of the anode should also be such that no hydrogen peroxide is produced as possible. Hydrogen peroxide has a significantly lower oxidation potential (1.8 V) and is therefore not sufficient for the destruction of some alkalizing agents. In addition, hydrogen peroxide (H 2 O 2 ) reacts with ozone to form short-lived OH radicals, delaying the destruction of the alkalizers due to the short-lived nature of OH radicals.
  • In the first process stage, therefore, according to the invention, a high current density is to be set in order to destroy the nitrogen-containing compounds by oxidation.
  • It turns out, however, that the destruction of nitrogen-containing impurities, such as ethanolamine, an increase of NH 4 and NO 3 is observed in the water. At the high current densities required for the first stage of the process, the total nitrogen content in the water is not reduced.
  • Surprisingly, it has been found that a reduction of the total nitrogen content by the formation of molecular nitrogen is possible when the electrochemical treatment is carried out with a lower current density at the diamond anode. Investigations have shown that it depends on an optimal ratio between produced at the anode ammonium and nitrate.
  • It has been found that the reaction process at the anode, for example, for ethanolamine as an alkalizing agent, for the formation of ammonium or - in further oxidation - can lead to the formation of nitrate. An essential parameter here is the current density. The complete oxidation at the anode therefore proceeds from the nitrogenous compound via ammonium to the nitrate. If all nitrogen-containing compounds are converted to nitrate, there is no reduction in the total nitrogen content.
  • On the other hand, if a setting is made in which ammonium and nitrate are formed in an optimum proportion to each other at the anode, the formation of molecular nitrogen due to this synproportionation, which can escape in gaseous form, reduces the total nitrogen content of the wastewater.
  • In the first stage of the process, care must therefore be taken to ensure that all nitrogen-containing compounds that form the contamination are destroyed, but that not too much nitrate is generated. Rather, the second process step must be initiated in good time, in which the adjustment of the low current density results in the setting of a defined and optimal ratio between produced ammonium and produced nitrate. The setting of the currents suitable for a used electrochemical treatment cell and the operating parameters used therein can be easily determined experimentally by measuring the concentrations of ammonium and nitrate. Furthermore, it is possible to determine the reduction of the total nitrogen content by the usual methods, wherein it should be noted that also the ion chromatography allows a rapid and meaningful determination of the total nitrogen content.
  • The duration of treatment in the first stage of the process depends on the load on the water with the nitrogen-containing compounds - and possibly additional organic constituents - that is on chemical oxygen demand (COD). In most applications, the user is aware of the COD content of his wastewater. Otherwise, the COD content can readily be determined by measuring methods known to those skilled in the art. It is essential that the charge entry into the wastewater is so high that all nitrogen-containing compounds are destroyed, but that a significant proportion of ammonium remains in the water and is not further oxidized to nitrate. The time of completion of the first stage of the process can easily be determined by measurements of the ammonium content and the nitrate content in a preliminary test so that the setting of the charge input at the selected current density (current intensity) can be determined so that a sufficient amount of ammonium remains in the wastewater , which in the second stage with the nitrate formed allows the formation of molecular nitrogen, thus contributing to the reduction of the total nitrogen content.
  • Examples
  • Example 1:
  • For the water treatment is suitable EP 1 730 080 B1 known electrode arrangement, as in 1 is shown schematically in exploded view. The electrode arrangement consists of an anode A, a cathode K and a conductive membrane M, which liquid-tightly seals an anode space AR with respect to a cathode space KR, wherein due to an open structure of the anode A and cathode K directly adjacent to the membrane M, the cathode space KR has a Side of the membrane M and the cathode K and the anode space AR with the opposite side of the membrane M and the anode A is formed. The membrane M is a conductive membrane, which ensures an ion transport by the folding of hydrogen bonds within the membrane M at waters of conductivity between 0.3 and 1000 μS / cm. Between the electrodes A, K and the membrane M, the charge is transferred via ion diffusion.
  • In a preferred embodiment, both electrodes, anode A and cathode K, are formed as diamond electrodes, wherein the base body of the electrodes A, K is an expanded metal grid. The expanded metal lattice leads to a rhombic formation of the electrode surface which abuts the membrane M with the tips of the rhombs ( 2 ). As a result, a region B with a high current density is formed around the tip in each case, in which ozone is predominantly formed at a suitable current intensity. At a greater distance from the membrane M forms an area in which the density of the OH radicals is lower, so that no longer from three OH radicals ozone, but only from two OH radicals hydrogen peroxide is formed. At an even greater distance from the membrane M, OH radicals are formed on the anode surface in a lower concentration, which thus react oxidatively with contaminants of the water which reach the surface of the anode A.
  • An increase in the conductivity of the water leads to an increase in the area in which hydrogen peroxide is formed. Since this is not desirable for the reasons mentioned above, the conductivity of the water should not be too large.
  • Example 2:
  • With an anode arrangement of Example 1, different treatment currents of 0.4 A, 1 A and 3 A have been realized. It turns out that, starting from the decomposition of ethanolamine (ETA), with the high current of 3 A, the total nitrogen is not reduced. With the current of 1 A, there is a slight reduction in the total nitrogen content, while a considerable reduction of the total nitrogen with the lower current of 0.4 A is possible with a relatively low charge input, as in 3 is shown. 4 illustrates the reduction of total nitrogen for the mentioned currents.
  • The mechanism for the degradation of total nitrogen is not fully understood. However, it appears that a reduction of the total nitrogen is due to a synproportionation of the oxidation products NH 4 and NO 3 , as this 5 shows. Thereafter, there is an optimum ratio of NO 3 and NH 4 for the formation of molecular (gaseous) N 2 . With increasing NO 3 content, the formation of N 2 decreases again after the optimum. Before the optimum, N 2 formation increases as the proportion of NO 3 to NH 4 increases .
  • It is therefore important to end the first stage of the process using the higher current density in good time so as not to make the proportion of NO 3 as the oxidation product too high.
  • The cathodic counter-reaction, in which NO 3 is first reduced to NH 4 , proceeds much more slowly, as the experiments according to this example have shown.
  • Example 3:
  • Examples 1 and 2 were carried out starting from the alkalizing agent ethanolamide. However, the process according to the invention is also suitable for correspondingly other alkalizing agents, such as, for example, morpholine, dimethylamine (DMA) and methoxypropylamine (MPA).
  • It has also been investigated whether it is possible to concentrate the wastewater contaminated with these alkalizing agents in order to be able to carry out the wastewater treatment according to the invention in smaller volumes of water.
  • 6 shows the degradation of the contemplated concentrates of the alkalizing agents ETA, DMA, MPA and morpholine. The concentrates can be completely degraded by the method according to the invention, as in 6 is shown. With the second method step according to the invention, the total nitrogen content can then be reduced.
  • With the method according to the invention, a reduction of the total nitrogen content of up to 72% has been achieved due to the second method step according to the invention. It is Thus, it is possible to effect both the destruction of the nitrogen-containing compounds and the reduction of the total nitrogen content in a common process with the two process steps. This represents a considerable simplification over the prior art.
  • QUOTES INCLUDE IN THE DESCRIPTION
  • This list of the documents listed by the applicant has been generated automatically and is included solely for the better information of the reader. The list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions.
  • Cited patent literature
    • US 5399247 [0002]
    • EP 1730080 B1 [0021]

Claims (6)

  1. Process for the oxidative degradation of nitrogen-containing compounds in wastewaters with the aid of an electrochemical treatment using a diamond electrode as the anode (A) and a cathode (K) as counterelectrode, characterized in that a first current density is set at the anode (A) in a first process stage is to oxidize the nitrogen-containing compounds and that subsequently with a second current density lower than the first current density, the total dissolved nitrogen content is reduced by release of molecular nitrogen.
  2. Method according to claim 1, characterized by the use of an anode body provided with a diamond layer, which abuts against a conductive membrane (M) in contact with the cathode (K) in order to form regions of high current density with conically tapered tips and an anode space ( AR) separated from a cathode space (KR) liquid-tight.
  3. A method according to claim 1 or 2, characterized by the use of an expanded metal grid as the anode body.
  4. Method according to one of claims 1 to 3, characterized by the use of an anode body of niobium or tantalum.
  5. Method according to one of claims 1 to 4, characterized by the use of a diamond electrode as a cathode.
  6. Method according to one of claims 1 to 5, characterized in that the nitrogen-containing compounds containing wastewater is concentrated prior to the electrochemical treatment.
DE102014002450.4A 2014-02-25 2014-02-25 Process for the oxidative degradation of nitrogenous compounds in waste water Withdrawn DE102014002450A1 (en)

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DE102014002450.4A DE102014002450A1 (en) 2014-02-25 2014-02-25 Process for the oxidative degradation of nitrogenous compounds in waste water
PCT/DE2015/000076 WO2015127918A1 (en) 2014-02-25 2015-02-11 Method for oxidative breakdown of nitrogenous compounds in waste water
CN201580009735.3A CN106458653A (en) 2014-02-25 2015-02-11 Method for oxidative breakdown of nitrogenous compounds in waste water
JP2016570159A JP2017512134A (en) 2014-02-25 2015-02-11 Method for oxidative degradation of nitrogen-containing compounds in wastewater
EP15713127.7A EP3110763A1 (en) 2014-02-25 2015-02-11 Method for oxidative breakdown of nitrogenous compounds in waste water

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JP (1) JP2017512134A (en)
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WO (1) WO2015127918A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102016119080A1 (en) 2016-10-07 2018-04-12 Condias Gmbh Apparatus for the electrochemical treatment of wastewater
DE102018131902B3 (en) * 2018-12-12 2020-02-27 Framatome Gmbh Process for conditioning ion exchange resins and device for carrying out the process

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US5399247A (en) 1993-12-22 1995-03-21 Eastman Kodak Company Method of electrolysis employing a doped diamond anode to oxidize solutes in wastewater
DE102004015680A1 (en) * 2004-03-26 2005-11-03 Condias Gmbh Electrode arrangement for electrochemical treatment of low conductivity liquids
EP2072472A1 (en) * 2007-12-19 2009-06-24 Condias Gmbh Method for performing an electro-chemical reaction and electro-chemical reactor arrangement
DE102008048691A1 (en) * 2008-07-07 2010-01-14 Areva Np Gmbh Process for conditioning a waste solution containing organic substances and metals in ionic form in wet-chemical cleaning of conventional or nuclear-engineering plants

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CN101234805A (en) * 2008-02-18 2008-08-06 中国矿业大学(北京) Highly effective denitrogenation electrochemical oxidation water treatment method and system
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CN202576055U (en) * 2012-05-21 2012-12-05 中国地质大学(北京) Device for performing electrochemical reduction on nitrate
CN103193301B (en) * 2013-04-27 2014-07-30 国电环境保护研究院 Electrochemical reactor for processing nitrogenous organic wastewater, and application and processing method thereof

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Publication number Priority date Publication date Assignee Title
US5399247A (en) 1993-12-22 1995-03-21 Eastman Kodak Company Method of electrolysis employing a doped diamond anode to oxidize solutes in wastewater
DE69410576T2 (en) * 1993-12-22 1999-02-04 Eastman Kodak Co Waste water treatment by electrolysis with a doped diamond anode
DE102004015680A1 (en) * 2004-03-26 2005-11-03 Condias Gmbh Electrode arrangement for electrochemical treatment of low conductivity liquids
EP1730080B1 (en) 2004-03-26 2008-01-16 Condias Gmbh Electrode assembly for the electrochemical treatment of liquids with a low conductivity
EP2072472A1 (en) * 2007-12-19 2009-06-24 Condias Gmbh Method for performing an electro-chemical reaction and electro-chemical reactor arrangement
DE102008048691A1 (en) * 2008-07-07 2010-01-14 Areva Np Gmbh Process for conditioning a waste solution containing organic substances and metals in ionic form in wet-chemical cleaning of conventional or nuclear-engineering plants

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102016119080A1 (en) 2016-10-07 2018-04-12 Condias Gmbh Apparatus for the electrochemical treatment of wastewater
US11008231B2 (en) 2016-10-07 2021-05-18 Condias Gmbh Apparatus for electrochemical treatment of wastewater
DE102018131902B3 (en) * 2018-12-12 2020-02-27 Framatome Gmbh Process for conditioning ion exchange resins and device for carrying out the process
WO2020120143A1 (en) 2018-12-12 2020-06-18 Framatome Gmbh Method for conditioning ion exchange resins and apparatus for carrying out the method

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WO2015127918A1 (en) 2015-09-03
EP3110763A1 (en) 2017-01-04
CN106458653A (en) 2017-02-22
JP2017512134A (en) 2017-05-18

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