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EP3230490A1 - Conduite de traitement optimisée pour le pré-traitement anti-corrosion du métal sur la base de bains riches en fluorure - Google Patents

Conduite de traitement optimisée pour le pré-traitement anti-corrosion du métal sur la base de bains riches en fluorure

Info

Publication number
EP3230490A1
EP3230490A1 EP15804502.1A EP15804502A EP3230490A1 EP 3230490 A1 EP3230490 A1 EP 3230490A1 EP 15804502 A EP15804502 A EP 15804502A EP 3230490 A1 EP3230490 A1 EP 3230490A1
Authority
EP
European Patent Office
Prior art keywords
titanium
mmol
water
pretreatment solution
soluble compounds
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.)
Withdrawn
Application number
EP15804502.1A
Other languages
German (de)
English (en)
Inventor
Jan-Willem Brouwer
Christian Stromberg
Frank-Oliver Pilarek
Jens KRÖMER
Fernando Jose RESANO ARTALEJO
Natascha HENZE
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.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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 Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP3230490A1 publication Critical patent/EP3230490A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/86—Regeneration of coating baths

Definitions

  • the present invention relates to a method for anticorrosive treatment, comprising a series of components with metallic surfaces of iron and / or zinc with a passivated aqueous pretreatment solution in a system tank containing compounds of zirconium and / or titanium and a source of fluoride ions in Contact is brought.
  • a passivated aqueous pretreatment solution in a system tank containing compounds of zirconium and / or titanium and a source of fluoride ions in Contact is brought.
  • a continuous, precise monitoring of the pretreatment processes is fundamentally crucial for the optimum dosing of the active components and possibly regulating chemicals in the surface treatment of metallic surfaces of components. This effort can only in modern production lines by a largely Automated monitoring and control of process chemicals dosing to maintain a long-lasting, optimal ratio of chemicals in process baths to meet the principles of material efficiency and consistent pre-treatment quality.
  • chromium (VI) compounds are finding increasingly less use, long known and established.
  • pretreatment solutions contain additional active components which are intended to further improve the anticorrosive action and paint adhesion.
  • EP 1 571 237 is cited, which is a
  • Pretreatment solution suitable for different metal surfaces containing up to 5000 ppm zirconium and / or titanium and up to 100 ppm free fluoride disclosed.
  • the solution may contain further components selected from chlorate, bromate, nitrite, nitrate, permanganate, vanadate, hydrogen peroxide, tungstate, molybdate or in each case the associated acids.
  • Organic polymers may also be present.
  • a pretreatment bath for producing a passivating conversion layer on metal surfaces therefore requires in individual cases a large number of active components which have to be regularly replenished during operation of a pretreatment bath. In order to achieve the highest possible material efficiency, there is a constant need for the
  • Pre-treatment process resource-saving, i. operate under conditions in which the use of active components can be reduced.
  • DE 10 2008 038653 discloses in this connection a method in which the active components which have been entrained into the sink with the component are cascaded back into the rinsing water before the actual pretreatment to produce a zirconium and / or titanium-based conversion layer.
  • the proportion of cascaded active components causes a partial passivation, which is completed in the subsequent pretreatment.
  • DE 10 2008 014465 reports, with regard to the corrosion protection treatment of metallic components by means of pretreatment solutions of fluorometalates of the elements zirconium and / or titanium, that the observance of an optimum molar ratio of fluoride ions to elements of the elements zirconium and / or titanium in serial
  • the fluoride scavengers are regulatory chemicals and in the specific case are preferably selected from compounds which release aluminum ions, calcium ions and / or iron ions.
  • the fluoride scavengers are regulatory chemicals and in the specific case are preferably selected from compounds which release aluminum ions, calcium ions and / or iron ions.
  • Treatment time of the metallic component may be.
  • Pretreatment solutions of fluorometalates of the elements zirconium and / or titanium can therefore only be ensured with a high level of analytical and process engineering effort, and last but not least, the use of considerable quantities of regulating chemicals.
  • the object of the present invention is thus, in the serial
  • a further object was to optimize the process so that a reliable corrosion-protective conversion based on the zirconium and / or titanium elements takes place, in particular, on the iron surfaces of the components treated in series, which are then used in conjunction with an organic primer coating or an organic primer coating Dip the high
  • This object is achieved by a method for corrosion protection treatment of a plurality of metallic surfaces of zinc and / or iron-containing components in series, in which each of these components with one located in a system tank
  • the passivating aqueous pretreatment solution comprises one or more water-soluble compounds of the elements zirconium and / or titanium and one or more water-soluble compounds which are a source of fluoride ions, and contacting for such a time that on the metallic surfaces of zinc and / or iron results in a layer of at least 0, 1 mmol / m 2 based on the elements zirconium and / or titanium, but none of these metallic surfaces has a layer coverage of more than 0.7 mmol / m 2 based on the elements zirconium and / or titanium, and wherein during the
  • Corrosion protection treatment of the components in series a part of the passivating aqueous pretreatment solution of the system tank is discarded and replaced by a sum of at least equal volume of one or more supplemental solutions by metering into the system tank in a manner that maintaining the concentration of the elements zirconium and / or Titanium in the passivating aqueous pretreatment solution in the form of water-soluble compounds, further characterized in that a concentration of zirconium and / or titanium in the passivating aqueous pretreatment solution in the form of water-soluble compounds of at least 0.05 mmol / L, but less than 0 in total , 8 mmol / L is maintained in the system tank, and the molar ratio of the total amount of fluorine in the form of water-soluble compounds, which are a source of fluoride ions (hereinafter "total amount of fluorine”), to the total amount of elements Z irconium and / or titanium in the form of water-soluble compounds (hereinafter "total
  • VW Ze ⁇ 2 ' 4 ,, 10 1 mmol m 2 (1)
  • VW throw on pretreatment solution in L / m 2 ;
  • the inventive method has the effect that the regulated Versch the free fluoride content in the pretreatment solution does not exceed values for which there is already a structural change of the conversion layer, which regularly with a
  • the throw of pretreatment solution for achieving the same purpose takes at least the following value:
  • VW 3 (Z f ⁇ 2 ' 4) 1 (T 1 mmol irr 2 , (T)
  • the throw is the liquid volume of pretreatment solution normalized to the unit surface (1 m 2 ) of the components to be treated which leaves the system tank during the serial pretreatment by passive extraction or due to a continuous or discontinuous overflow per square meter of a treated component.
  • a pre-treatment in series according to the present invention is when a plurality of components is brought into contact with the pre-treatment solution in the system tank, whereby the individual components are brought into contact one after the other and thus separated in time.
  • the system tank is the container in which the pretreatment solution is in series for the purpose of passivating pretreatment.
  • the area to be set in the method according to the invention for the layer support based on the elements Zr and / or Ti can be determined by means of X-ray fluorescence analysis (RFA) after calibration on the basis of solutions of known molarity of H ZrFö and F TiFö in the dry-in-place method coated metal surfaces.
  • the solutions of known molarity are applied to produce the calibration sample plates in a defined wet film thickness and the wet film is then completely dried.
  • the determination of the actual layer support according to the present invention can be based on this
  • Solubility in deionized water having a conductivity of not more than 1 Sc a temperature of 20 ° C is at least 1 g / l.
  • Total amount of fluorine to the total amount of the elements zirconium and / or titanium in the added total volume of the replenisher is therefore not less than 5.0, more preferably not less than 5.5.
  • selbiges ratio in the total volume of the added dose replenishers smaller in the inventive method as a ⁇ '4 "1" 1 L + 6, or alternatively, less than 9.25 is
  • the inventive method makes due to the controlled Versches
  • the minimum throw is for the given conditions with respect to the concentration of active components in the pretreatment solution and the planned coating layer of a maximum of 0.7 mmol / m 2 based on the elements zirconium and titanium according to the semi-empirically found term (1) or the preferred semi adjust -empirischen Terme (V) and (1 ").
  • These terms for the technicianvermine are only of the specific concentration of zirconium and / or titanium in the pretreatment solution and the ratio of the elements fluorine in the form of dissolved in water compounds to the total amount of zirconium and / or titanium in the form of compounds dissolved in water in the supplement solution.
  • Conversion layer training is regularly check.
  • the monitoring of the amount of free fluoride in the pretreatment solution becomes unnecessary in the process according to the invention.
  • Pretreatment solution can be dispensed with, their proportion in accordance with the inventionopteddos faced volume of the supplementary solution for reasons of material efficiency is low.
  • processes according to the invention are preferably processes for which the molar ratio of the total amount of the elements zirconium and / or titanium in each case to the total amount of one of the elements calcium, magnesium, aluminum, boron, iron, manganese or tungsten in the form of water-soluble compounds in the added total volume of the supplementary solution is greater is 5: 1, more preferably greater than 10: 1.
  • a further advantage of the method according to the invention is that sufficient coating deposits of zirconium and / or titanium are already achieved with relatively low concentrations of active components for corrosion protection and adhesion to a subsequently applied organic primer.
  • those methods according to the invention are preferred for material efficiency in which the passivating aqueous pretreatment solution in the system tank is less than 0.65 mmol / L, more preferably less than 0.55 mmol / L, most preferably less than 0.325 mmol / L of water-soluble compounds of the elements zirconium and / or titanium.
  • a low concentration of active components also causes the stationary by being carried over into a downstream sink introduced proportion of these compounds is low.
  • passivating aqueous pretreatment solution is not greater than the following value in liters per massively treated square meter of metallic component:
  • VW throw on pretreatment solution in order 2 ;
  • C SS 6 concentration of zirconium and / or titanium in the pretreatment solution in mmol / L;
  • the pH of the passivating aqueous pretreatment solution in a preferred process according to the invention is not less than 3.0, more preferably not less than 3.5, but preferably not greater than 5.0, more preferably not greater than 4.5.
  • the “pH value” according to the present invention corresponds to the negative logarithm of the hydronium ion activity at 20 ° C. and can be determined by means of a pH-sensitive glass electrode.
  • the process of the invention is preferably at relatively low
  • the temperature of the passivating aqueous pretreatment solution is not greater than 45 ° C, more preferably not greater than 40 ° C, most preferably not greater than 35 ° C.
  • the Versch provided in pretreatment solution according to the invention can be carried out during the corrosion protection treatment of the plurality of components process-related only quasi-continuous or discontinuous.
  • the inventive process of the series treatment requires that with each treated component a certain amount of pretreatment solution irrevocably leaves the system tank.
  • the amount of rejects entrained with each treated component is inherently discrete and therefore discontinuous and dependent on the specific treatment conditions and the geometry of the components.
  • the dragged portion of Versch is only partially accessible to a scheme, for example, by rotation or tilting of the components in the
  • the rejection of the passivating aqueous pretreatment solution preferably takes place both by extracting the pretreatment solution with each component of the series of components to be treated and by actively discharging
  • Pretreatment solution in each case from the system tank of pretreatment.
  • Pretreatment solution to the deposited in the pretreatment step on the components layer support with respect to the elements zirconium and / or titanium adjusted to redesignspeisen for a desired coating layer of zirconium and / or titanium as much as necessary, but not more than necessary to pretreatment solution and on to do this as economically as possible.
  • discontinuous operation such methods are preferred in which the discontinuous Versch VWd is carried out on passivating aqueous pretreatment solution after pretreatment of a certain number n of components i, wherein the
  • discontinuous throw at least the following value in liters for a series treated number n of components i assumes:
  • VW d discontinuous throw in liters
  • VW a n Rejected by removal by n components in liters with the proviso that
  • xp 5 proportion of iron surface area relative to the total surface area of zinc and iron of the ith series-treated component
  • A total area of metallic surfaces of zinc and iron of the ith series-treated component
  • n positive natural number ⁇ n e N n> 1 ⁇
  • Total amount of elements zirconium and / or titanium in the supplementary solution satisfies the following condition:
  • the throwing by active feeding of passivating aqueous pretreatment solution and the replacement of discarded pretreatment solution with replenisher are carried out continuously during the pretreatment of the components in series, more preferably by feeding a constant volume flow of replenishing replacer solution into the system tank of the pretreatment, wherein the continuous Versch at passivating aqueous pretreatment solution is preferably realized mainly by overflowing an open system tank.
  • Predominantly in this context means that more than 50%, preferably more than 80%, of the control accessible portion of the discarded pretreatment solution is not the inevitable part due to the scavenging effect of the components or the wet film adhered to the components
  • the overflow is thus a particularly preferred type of Ver Dahles by active Ausspeisen.
  • the overflow can be removed by an overflow from the system tank
  • continuous Versch also be realized by feeding a constant volume flow from the system tank.
  • the continuous throw assumes at least the following value in liters per square meter of metallic surfaces of zinc and iron treated in order to obtain as much as required, but not more than, 20,000 for a coating of zirconium and / or titanium to be achieved necessary
  • x average proportion of iron surfaces in relation to the total surface area of zinc and iron of a series of treated components
  • Preferred upper limits for the continuously discharged pretreatment solution are processes according to the invention in which the continuous throw in liters per per square meter of metallic surfaces of zinc and iron treated in series has the value
  • VW C ⁇ - (x S + x S) A - VW a (6)
  • Total amount of elements zirconium and / or titanium in the supplementary solution satisfies the following condition:
  • ) with knowledge of the bath concentration of zirconium and / or titanium is sufficient to specify on the setting of the continuous or discontinuous Versches the target state with respect to layer support for other components and an optimally protected against corrosion Lackhaftground.
  • an effective scheme that only monitoring the amount of zirconium and / or titanium in the
  • ) based on the elements zirconium and / or titanium can be determined immediately after the pretreatment of the component by means of X-ray fluorescence analysis on the respective treated metal surface as described above.
  • the discontinuous Versch is carried out immediately after the first rinse, wherein the first sink preferably by means of a
  • wet holding ring is made by spraying the components with the first rinse water, wherein the rinse water is again preferably at least partially fed as part of the supplement solution in the pretreatment solution.
  • Pretreatment solution on the regulation of Verdeses based on the layer support can be made almost immediately.
  • the Versch occurs quasi-continuously or if possible discontinuously as possible after each pretreatment of only a small number n of components.
  • VW C Ze ⁇ 2 ' 4 ,, O / lmmoIrrT 2 - ⁇ - VW a (5 ' )
  • VW C • 0.7 mmolm ⁇ 2 ⁇ A - VW a (5 "' )
  • VW C , VWd discontinuous or continuous Ver Dahles
  • At least 80% of the surfaces of the component will be formed by surfaces of the substrates iron, zinc and aluminum, more preferably at least 50% of the surfaces of the component being metallic surfaces of the substrates iron and / or zinc, again preferably at least 10%, particularly preferably at least 20%, of the metallic surfaces of the component are selected from surfaces of the substrate iron.
  • the surfaces of the substrates iron, zinc and aluminum are also their
  • the process of the invention may be further process steps for
  • Binder system preferably a powder coating or dip coating, more preferably an electrocoating, particularly preferably a cathodic electrodeposition coating.
  • an electrocoating particularly preferably a cathodic electrodeposition coating.
  • subsequent dip coating in particular a subsequent electrocoating, takes place after contacting with the passivating aqueous pretreatment solution and before dip coating
  • a drying step is characterized by performing technical measures for drying the surfaces of the component, for example, by supplying thermal energy or by supplying a dry air flow.
  • Metal surface of the component to form a coating containing substrate-foreign metallic or semi-metallic elements with a layer support of more than 0.1 mmol / m 2 based on these substrate-foreign elements.
  • Pretreatment Solution is any element that is not the main alloying element of the substrate in question.
  • a rinsing step is carried out by bringing the components into contact with a system tank
  • Rinsing solution wherein during the anticorrosive treatment of the components in series part of the rinse solution discarded and replaced by an at least equal volume of a supplementary rinse solution, the total less than 10 "5 mol / L on
  • water-soluble compounds of the elements zirconium and / or titanium and preferably less than 10.sup.- 4 mol / l of water-soluble compounds which are a source of fluoride ions, based on the element fluorine Active components from the passivating aqueous pretreatment solution in the rinse solution is tolerated only to a certain extent, since otherwise damage to the passive layer can not be completely ruled out.
  • the throw of rinsing solution per treated in series total surface area of the components is less than 2 liters / m 2 .
  • this upper limit can always be maintained without additional measures for working up the
  • Rinsing solution would be necessary. It is further preferred if at least a portion of the discarded rinsing solution is fed as a replenisher into the system tank of the passing aqueous pretreatment, wherein regularly additionally the dosage of a concentrated
  • the water-soluble compounds of the elements zirconium and / or titanium are therefore not restricted to any particular class of compounds both in the pretreatment solution and in the supplemental solutions, but preferred are oxyfluorides of the respective elements, particularly preferably the fluoroacids and salts thereof.
  • oxyfluorides of the respective elements particularly preferably the fluoroacids and salts thereof.
  • basic zirconium carbonate or titanyl sulfate these compounds then having to be reacted with a corresponding amount of fluoride-releasing compounds because of the ratio of fluorides dissolved in water according to the invention to compounds of zirconium and / or titanium dissolved in water in order to form an adequate supplementary solution.
  • Water-soluble compounds which are a source of fluoride ions and to which extent the process according to the invention can be based are, for example, hydrofluoric acid, ammonium bifluoride and sodium fluoride or the abovementioned oxyfluorides and fluoro acids of the elements zirconium and / or titanium.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

La présente invention concerne un procédé de traitement anti-corrosion, au cours duquel une série de composants disposant d'une surface métallique en fer et/ou en zinc est amenée en contact avec une solution de prétraitement aqueuse passive contenant un mélange d'éléments de zirconium et/ou de titane se trouvant dans un réservoir principal ainsi qu'une source d'ions fluorure. L'invention concerne un procédé visant à retirer une partie de cette solution de prétraitement et de la remplacer par une quantité au moins égale en volume d'une ou de plusieurs solutions de remplacement par addition dans le réservoir principal de prétraitement. Au cours du retrait, en fonction du rapport molaire du fluorure par rapport au zirconium et/ou au titane, une valeur prédéterminée ne doit pas être dépassée pour garantir un traitement anti-corrosion satisfaisant et durable, même en cas de renoncement total à l'utilisation de produits chimiques pour la régulation du taux de décapage ou la stabilisation du chargement en ions. A cet effet, l'addition de la solution complémentaire a lieu de telle façon qu'un maintien de la concentration des éléments de zirconium et/ou de titane est garanti dans la solution de prétraitement aqueuse passive sous forme de composés solubles dans l'eau.
EP15804502.1A 2014-12-12 2015-12-03 Conduite de traitement optimisée pour le pré-traitement anti-corrosion du métal sur la base de bains riches en fluorure Withdrawn EP3230490A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP14197667.0A EP3031951B1 (fr) 2014-12-12 2014-12-12 Traitement optimisé dans le pré-traitement du métal contre la corrosion à base de bains contenant du fluorure
PCT/EP2015/078511 WO2016091713A1 (fr) 2014-12-12 2015-12-03 Conduite de traitement optimisée pour le pré-traitement anti-corrosion du métal sur la base de bains riches en fluorure

Publications (1)

Publication Number Publication Date
EP3230490A1 true EP3230490A1 (fr) 2017-10-18

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Family Applications (2)

Application Number Title Priority Date Filing Date
EP14197667.0A Active EP3031951B1 (fr) 2014-12-12 2014-12-12 Traitement optimisé dans le pré-traitement du métal contre la corrosion à base de bains contenant du fluorure
EP15804502.1A Withdrawn EP3230490A1 (fr) 2014-12-12 2015-12-03 Conduite de traitement optimisée pour le pré-traitement anti-corrosion du métal sur la base de bains riches en fluorure

Family Applications Before (1)

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EP14197667.0A Active EP3031951B1 (fr) 2014-12-12 2014-12-12 Traitement optimisé dans le pré-traitement du métal contre la corrosion à base de bains contenant du fluorure

Country Status (13)

Country Link
US (1) US10458022B2 (fr)
EP (2) EP3031951B1 (fr)
JP (1) JP6720175B2 (fr)
KR (1) KR102504477B1 (fr)
CN (1) CN107002245B (fr)
BR (1) BR112017012144B1 (fr)
CA (1) CA2970405A1 (fr)
ES (1) ES2654893T3 (fr)
HU (1) HUE036114T2 (fr)
MX (1) MX375812B (fr)
PL (1) PL3031951T3 (fr)
TW (1) TWI678434B (fr)
WO (1) WO2016091713A1 (fr)

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CN110129783A (zh) * 2019-04-15 2019-08-16 汉腾汽车有限公司 一种涂装前处理工艺

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Also Published As

Publication number Publication date
CA2970405A1 (fr) 2016-06-16
EP3031951A1 (fr) 2016-06-15
JP2017537229A (ja) 2017-12-14
BR112017012144A2 (pt) 2018-01-02
HUE036114T2 (hu) 2018-06-28
US10458022B2 (en) 2019-10-29
TW201631212A (zh) 2016-09-01
TWI678434B (zh) 2019-12-01
JP6720175B2 (ja) 2020-07-08
US20170283955A1 (en) 2017-10-05
ES2654893T3 (es) 2018-02-15
MX375812B (es) 2025-03-07
CN107002245B (zh) 2019-04-09
WO2016091713A1 (fr) 2016-06-16
KR102504477B1 (ko) 2023-02-28
MX2017007556A (es) 2017-10-31
EP3031951B1 (fr) 2017-10-04
KR20170110575A (ko) 2017-10-11
PL3031951T3 (pl) 2018-03-30
CN107002245A (zh) 2017-08-01
BR112017012144B1 (pt) 2021-06-22

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