WO2015199224A1 - イオン交換樹脂及び金属の吸着分離方法 - Google Patents

イオン交換樹脂及び金属の吸着分離方法 Download PDF

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Publication number
WO2015199224A1
WO2015199224A1 PCT/JP2015/068520 JP2015068520W WO2015199224A1 WO 2015199224 A1 WO2015199224 A1 WO 2015199224A1 JP 2015068520 W JP2015068520 W JP 2015068520W WO 2015199224 A1 WO2015199224 A1 WO 2015199224A1
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WIPO (PCT)
Prior art keywords
ion exchange
exchange resin
rare earth
metal
adsorbed
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.)
Ceased
Application number
PCT/JP2015/068520
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English (en)
French (fr)
Japanese (ja)
Inventor
後藤　雅宏
富生子 久保田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Metal Mining Co Ltd
Kyushu University NUC
Original Assignee
Sumitomo Metal Mining Co Ltd
Kyushu University NUC
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sumitomo Metal Mining Co Ltd, Kyushu University NUC filed Critical Sumitomo Metal Mining Co Ltd
Priority to CA2954605A priority Critical patent/CA2954605C/en
Priority to AU2015281011A priority patent/AU2015281011B2/en
Priority to US15/321,286 priority patent/US9863018B2/en
Priority to EP15810881.1A priority patent/EP3156128B1/en
Publication of WO2015199224A1 publication Critical patent/WO2015199224A1/ja
Priority to PH12016502610A priority patent/PH12016502610A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J45/00—Ion-exchange in which a complex or a chelate is formed; Use of material as complex or chelate forming ion-exchangers; Treatment of material for improving the complex or chelate forming ion-exchange properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J47/00—Ion-exchange processes in general; Apparatus therefor
    • B01J47/12—Ion-exchange processes in general; Apparatus therefor characterised by the use of ion-exchange material in the form of ribbons, filaments, fibres or sheets, e.g. membranes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/28—Amines
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/32—Carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00—Obtaining rare earth metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to an ion-exchange resin and a metal adsorption / separation method.
  • Cobalt and rare earth metals are known as valuable metals and are used for various purposes in industry. Cobalt is used in superalloys (high-strength heat-resistant alloys) used for aircraft jet engines and the like, in addition to positive electrode materials for secondary batteries. Rare earth metals are used in phosphor materials, negative electrodes for nickel metal hydride batteries, additives for magnets mounted on motors, abrasives for glass substrates used in liquid crystal panels and hard disk drives, and the like.
  • a wet method in which a used battery is dissolved in an acid and a metal is recovered using a separation method such as a precipitation method, a solvent extraction method, or electrolytic collection.
  • a precipitation method there are a method of adjusting the pH of a solution containing cobalt and manganese, a method of obtaining a cobalt sulfide starch by adding a sulfurizing agent, and a method of obtaining a manganese oxide starch by adding an oxidizing agent. It is known (see, for example, Patent Document 1).
  • this method has problems such as coprecipitation, and it is difficult to completely separate cobalt and manganese.
  • an acidic extractant is widely used.
  • the battery solution contains a high concentration of manganese. There is no effective extractant to extract effectively.
  • cobalt smelting currently used to produce cobalt is made of nickel ore such as nickel oxide ore, but nickel oxide ore has a manganese ratio compared to cobalt. It is high, and its abundance ratio is about 5 to 10 times that of cobalt, and separation of manganese is a major issue when smelting cobalt.
  • a mixture of rare earth metals such as lanthanum, cerium, yttrium, terbium and europium is used for the phosphor used in the three-wavelength fluorescent tube mentioned above.
  • the phosphor for a cathode ray tube contains yttrium and europium together with a high ratio of zinc.
  • a method of recovering a specific rare earth metal from a mixture of rare earth metals a method of recovering from a solution dissolved in an acid such as mineral acid by a solvent extraction method is generally used.
  • a trade name PC88A manufactured by Daihachi Chemical
  • this extractant contains phosphorus in its structure, advanced wastewater treatment is required to prevent contamination of public water areas by extractants and their degradation products that migrate into wastewater when used industrially. It becomes.
  • the total amount regulation stipulated by the Water Pollution Law which is a concern when used on an industrial scale.
  • a carboxylic acid-based extractant for example, 2-methyl-2-ethyl-1-heptanoic acid: neodecanoic acid
  • this extraction agent can be extracted only in a pH range higher than neutrality, when targeting an acidic solution as described above, a large amount of neutralizing agent is required and there is a concern about an increase in cost.
  • the extraction capacity of the carboxylic acid-based extractant is lower than that of the above-described phosphorus-based extractant, and excessive equipment is required, which increases the cost.
  • DODGAA having a diglycolamide acid skeleton
  • Patent Document 2 an extractant called DODGAA having a diglycolamide acid skeleton
  • Y yttrium
  • Lu lutetium
  • Yb ytterbium
  • Tm thulium
  • Er erbium
  • Ho Holmium
  • Dy dysprosium
  • Tb terbium
  • Gd gadolinium
  • Eu europium
  • Sm samarium
  • the concentration of scandium contained in the acid solution is about several to several tens mg / l, which is extremely dilute.
  • the concentration of scandium contained in the acid solution is extremely dilute, so that a large amount of extractant is required for the solvent extraction treatment.
  • the scale of equipment such as extraction tanks and liquid storage tanks is increased corresponding to the large amount of extractant, and the necessary capital investment is increased.
  • the extraction characteristics tend to fluctuate and stable operation becomes difficult. Management is required.
  • iron ions contained in the solution are oxidized to produce inclusions called clads, which may hinder the solvent extraction operation.
  • the acid solution obtained by acid leaching the nickel oxide ore often contains divalent iron ions at a high concentration of several g / l or more, and the concentration of the divalent iron ions contained in the acid solution can be set as much as possible. It is preferable to carry out the solvent extraction process after keeping it low.
  • the object of the present invention is to provide a system for efficiently recovering trace metals from a large amount of raw materials as in the case of recovering trace metals from nickel oxide ore.
  • the present invention provides the following.
  • the present invention is an ion exchange resin having an amide derivative represented by the following general formula (I) on a carrier.
  • R1 and R2 each represent the same or different alkyl group.
  • the alkyl group may be linear or branched.
  • R3 represents a hydrogen atom or an alkyl group.
  • R4 represents a hydrogen atom or an amino acid as ⁇ . An arbitrary group other than an amino group bonded to carbon is shown.
  • this invention is an ion exchange resin as described in (1) whose said amide derivative is a glycinamide derivative.
  • this invention is an ion exchange resin as described in (1) or (2) in which the said support
  • one or more metals selected from cobalt, nickel, scandium, and rare earth elements are adsorbed to the resin according to any one of (1) to (3), and adsorbed to the resin. This is a metal adsorption separation method for recovering metal.
  • the ion exchange resin of the present invention has an amide derivative represented by the following general formula (I) on a carrier.
  • a carrier for introducing an alkyl group into the skeleton of the amide, the lipophilicity is enhanced and it can be used as a functional group when adsorbing one or more metals selected from cobalt, nickel, scandium and other rare earth elements. .
  • the type of ion exchange resin suitably adsorbs trace metals (one or more trace metals selected from cobalt, nickel, scandium and other rare earth elements) contained in an acid leaching solution such as nickel oxide ore, and subsequent treatment. There is no particular limitation as long as the metal adsorbed on the resin can be suitably recovered.
  • the solid extractant such as an ion exchange resin can be handled physically and stably, can be operated with a simple apparatus, and has an advantage that it can be separated relatively stably even with fluctuations in operating conditions.
  • the reaction by ion exchange has little physical movement such as mixing the extraction agent and the solution as in the solvent extraction method, and the contact between the ion exchange resin and the solution is generally performed in a sealed column. In many cases, air is prevented from being involved, and as a result, generation of clad is suppressed and operation is stably performed.
  • the substituents R1 and R2 each represent the same or different alkyl group.
  • the alkyl group may be linear or branched.
  • the number of carbon atoms of the alkyl group is not particularly limited, but is preferably 5 or more and 11 or less.
  • R3 represents a hydrogen atom or an alkyl group.
  • R4 represents a hydrogen atom or any group other than an amino group bonded to the ⁇ -carbon as an amino acid.
  • the type of the amide derivative is not particularly limited as long as it can adsorb one or more metals selected from cobalt, nickel, scandium, and other rare earth elements, but is a glycinamide derivative in that it can be easily produced. It is preferable that When the amide derivative is a glycinamide derivative, the above glycinamide derivative can be synthesized by the following method. First, 2-halogenated acetyl halide is added to an alkylamine having a structure represented by NHR1R2 (R1 and R2 are the same as the above substituents R1 and R2), and the hydrogen atom of the amine is converted to 2-halogen by a nucleophilic substitution reaction. Substitution with acetyl chloride gives 2-halogenated (N, N-di) alkylacetamide.
  • histidine amide derivatives by replacing glycine with histidine, lysine, and aspartic acid, histidine amide derivatives, lysine amide derivatives, and aspartic acid amide derivatives can be synthesized.
  • the carrier is capable of binding the above amide derivative and is chemically stable in the acidic solution to be adsorbed and is not physically affected when placed in a column or solution, and deteriorates during the adsorption operation. It is not particularly limited as long as it is a solid material that does not.
  • the support preferably contains a primary amine and / or a secondary amine.
  • the carrier preferably contains a primary amine so that the target trace metal can be selectively adsorbed.
  • the carrier examples include 3-aminopropyl silica gel, 3- (ethylenediamino) propyl silica gel and the like.
  • the pH of the acidic solution is preferably 3.5 or more and 5.5 or less, and preferably 4.0 or more and 5.0 or less. More preferred. If the pH is less than 3.5, cobalt may not be sufficiently adsorbed. When the pH exceeds 5.5, not only cobalt but also manganese may be adsorbed.
  • the pH of the acidic solution is preferably 0.5 or more and 2.5 or less, more preferably 1.0 or more and 2.0 or less. More preferably, it is 5 or more and 2.0 or less. If the pH is less than 0.5, scandium may not be sufficiently adsorbed. When the pH exceeds 2.5, for example, when the acidic solution is an acidic solution obtained by acid leaching of nickel oxide ore, not only scandium but also aluminum, zinc, nickel, cobalt, etc. contained in the acidic solution are adsorbed. There is a possibility that it will be necessary to purify in a later step, and the labor may be increased.
  • the pH of the acidic solution is preferably 2.0 or more and 3.0 or less. If the pH is less than 2.0, europium may not be sufficiently extracted. When the pH exceeds 3.0, not only europium but also other rare earth metals such as yttrium may be adsorbed.
  • the ion exchange resin or the like of the present invention is characterized in that light rare earth elements and medium rare earth elements are more easily adsorbed than heavy rare earth elements. Therefore, light rare earth elements can be selectively adsorbed from the solution by contacting with the ion exchange resin of the present invention while adjusting the pH of the solution containing both heavy rare earth elements and light rare earth elements. As a result, light rare earth elements and heavy rare earth elements can be separated.
  • the eluent recovered from the ion exchange resin or the like by the method described in ⁇ Recovery of valuable metal from resin> is, for example, the above general formula (I)
  • the light rare earth element and the medium rare earth element can be suitably separated by subjecting to solvent extraction using an organic solvent containing an amide derivative represented by the formula:
  • the pH of the acidic solution is preferably 1.7 or more and 2.7 or less. If the pH is less than 1.7, light rare earth elements may not be sufficiently adsorbed. If the pH exceeds 2.7, not only light rare earth elements but also heavy rare earth elements may be adsorbed.
  • the ion exchange resin after adsorbing valuable metal ions is cleaned of the ion exchange resin with pure water or the like to remove a part of the acidic solution adhering to the surface, as is conventionally known. Subsequently, the target valuable metal ions can be recovered from the ion exchange resin by passing an eluent whose pH is adjusted lower than that of the acidic aqueous solution.
  • the eluent is not particularly limited as long as the pH is adjusted to be lower than that of the acidic aqueous solution, and examples thereof include an aqueous solution diluted with nitric acid, hydrochloric acid, and sulfuric acid. Further, the target valuable metal ions can be concentrated by appropriately changing the contact time between the ion exchange resin and the eluent, that is, the passage time through the column.
  • the liquid passing speed and the liquid temperature may be appropriately set depending on the acidic aqueous solution of the valuable metal ions and the conditions since the equilibrium time varies depending on the type and concentration of the valuable metal.
  • the pH of the acidic aqueous solution containing metal ions can also be adjusted as appropriate depending on the type of valuable metal.
  • An ion exchange resin having D2EHAG was prepared as follows. (1) 4.37 g of chloroacetyl chloride (corresponding to 3 equivalents relative to the amine of silica gel to be supported) and 1.32 g of triethylamine (TEA) were separated, and dissolved by adding 70 ml of dichloromethane (DCM). (2) To the solution obtained in (1), 10 g of 3-aminopropyl silica gel was added and stirred for a whole day and night while maintaining at room temperature. (3) After stirring, the product was filtered and washed with methanol. (4) After washing, drying was performed to obtain about 10 g of an intermediate silica gel having a light yellow color. The recovery rate calculated from the quantity was about 92%.
  • Example 2 An ion exchange resin (glycine aceto (ethylenediamino) propyl silica gel) according to Example 2 was obtained in the same manner as in Example 1 except that 3-aminopropyl silica gel was changed to 3- (ethylenediamino) propyl silica gel. .
  • glycinamide derivatives normal-methyl glycine derivatives, histidine amide derivatives, and the like are known as amide derivatives. These are also supported as functional groups on a carrier in the same manner as in the case of glycinamide derivatives, It can be an exchange resin.
  • the ion exchange resin and the solution after adsorption were separated into solid and liquid using a filter paper, and the pH of the solution after adsorption was measured.
  • a small amount of pure water is used to wash the ion-exchange resin with water, and the post-adsorption liquid and the wash water are combined to measure the volume as a new post-adsorption liquid, and an induction plasma emission spectrometer (ICP-AES) is installed. The concentration in the post-adsorption liquid of the components contained in the starting liquid was measured.
  • ICP-AES induction plasma emission spectrometer
  • the adsorption rate (distribution) to the ion exchange resin was defined by (1-quantity after adsorption / quantity before adsorption) from the change in the quantity of the acidic solution before and after adsorption.
  • the results for Example 1 are shown in Table 1 and FIG. 1, and the results for Example 2 are shown in Table 2 and FIG. 1 and 2, the horizontal axis represents the pH of the acidic solution, and the vertical axis represents the extraction rate (unit:-) of various metal elements.
  • one or more metals selected from cobalt, nickel, scandium and rare earth elements can be obtained by suitably adjusting the pH of the acidic solution. It was confirmed that selective adsorption was possible. Moreover, from this result, the metal (one or more metals selected from cobalt, nickel, scandium and rare earth elements) contained in the acid leaching solution obtained by high-temperature pressure acid leaching of nickel oxide ore can be selectively adsorbed. I can say that.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
PCT/JP2015/068520 2014-06-26 2015-06-26 イオン交換樹脂及び金属の吸着分離方法 Ceased WO2015199224A1 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CA2954605A CA2954605C (en) 2014-06-26 2015-06-26 Ion exchange resin and method for adsorbing and separating metal
AU2015281011A AU2015281011B2 (en) 2014-06-26 2015-06-26 Ion exchange resin and method for adsorbing and separating metal
US15/321,286 US9863018B2 (en) 2014-06-26 2015-06-26 Ion exchange resin and method for adsorbing and separating metal
EP15810881.1A EP3156128B1 (en) 2014-06-26 2015-06-26 Ion exchange resin and method for adsorbing and separating metal
PH12016502610A PH12016502610A1 (en) 2014-06-26 2016-12-23 Ion exchange resin and method for adsorbing and separating metal

Applications Claiming Priority (2)

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JP2014-131673 2014-06-26
JP2014131673A JP6053724B2 (ja) 2014-06-26 2014-06-26 イオン交換樹脂及び金属の吸着分離方法

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US (1) US9863018B2 (enExample)
EP (1) EP3156128B1 (enExample)
JP (1) JP6053724B2 (enExample)
AU (1) AU2015281011B2 (enExample)
CA (1) CA2954605C (enExample)
PH (1) PH12016502610A1 (enExample)
WO (1) WO2015199224A1 (enExample)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20190040492A1 (en) * 2016-02-05 2019-02-07 Sumitomo Metal Mining Co., Ltd. Method for recovering scandium

Families Citing this family (3)

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Publication number Priority date Publication date Assignee Title
JP6638939B2 (ja) * 2016-03-30 2020-02-05 株式会社Ｇｓユアサ 亜鉛電極、及びその亜鉛電極を備えた蓄電池
JP7274171B2 (ja) * 2019-05-31 2023-05-16 国立研究開発法人産業技術総合研究所 希土類元素の吸着剤、及び希土類元素の分離方法
JP7249317B2 (ja) * 2020-08-07 2023-03-30 株式会社 イージーエス 金属の分離方法、および、金属の分離装置

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JPH0597715A (ja) * 1991-10-09 1993-04-20 Eisai Co Ltd コンアルブミンが結合した光学異性体分離剤
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CA2954605C (en) 2018-01-23
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EP3156128A4 (en) 2017-06-14
JP6053724B2 (ja) 2016-12-27
AU2015281011A1 (en) 2017-01-19
PH12016502610B1 (en) 2017-04-24
EP3156128B1 (en) 2019-03-20
EP3156128A1 (en) 2017-04-19
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