EP3449040A1 - Composition permettant de réduire l'enlèvement par décapage lors du décapage de surfaces métalliques contenant de l'acier nu et/ou galvanisé - Google Patents

Composition permettant de réduire l'enlèvement par décapage lors du décapage de surfaces métalliques contenant de l'acier nu et/ou galvanisé

Info

Publication number
EP3449040A1
EP3449040A1 EP17721118.2A EP17721118A EP3449040A1 EP 3449040 A1 EP3449040 A1 EP 3449040A1 EP 17721118 A EP17721118 A EP 17721118A EP 3449040 A1 EP3449040 A1 EP 3449040A1
Authority
EP
European Patent Office
Prior art keywords
pickling
composition
formula
range
compound
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.)
Granted
Application number
EP17721118.2A
Other languages
German (de)
English (en)
Other versions
EP3449040B1 (fr
Inventor
Anna Verena MOHR
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.)
Chemetall GmbH
Original Assignee
Chemetall GmbH
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 Chemetall GmbH filed Critical Chemetall GmbH
Priority to PL17721118T priority Critical patent/PL3449040T3/pl
Publication of EP3449040A1 publication Critical patent/EP3449040A1/fr
Application granted granted Critical
Publication of EP3449040B1 publication Critical patent/EP3449040B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
    • C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
    • C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
    • C23G1/065—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors sulfur-containing compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/28—Acidic compositions for etching iron group metals
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
    • C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
    • C23G1/061—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors nitrogen-containing compounds
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
    • C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
    • C23G1/068—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors compounds containing a C=C bond
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • C23G1/081—Iron or steel solutions containing H2SO4
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/19—Iron or steel
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/24—Cleaning or pickling metallic material with solutions or molten salts with neutral solutions
    • C23G1/26—Cleaning or pickling metallic material with solutions or molten salts with neutral solutions using inhibitors

Definitions

  • the invention relates to an aqueous composition for reducing pickling during pickling of metallic surfaces containing bare and / or galvanized steel and to a process for pickling a corresponding metallic surface with reduced pickling.
  • Atmospheric corrosion or heat treatment e.g., heat generation during forming or welding
  • pickling means the dissolution of these oxide layers in mineral acid solutions in order to achieve a metallically clean surface for further processing.
  • This essentially serves to remove oxide films of rust - FeO, Fe 2 O 3 , Fe 3 O 4 and iron oxide hydrates - or zinc oxide from the surface, which in turn increases the adhesive strength and uniformity of subsequent coatings, in particular a conversion coating on the surface.
  • the object of the invention was therefore to provide a composition for reducing pickling during pickling of metallic surfaces containing bare and / or galvanized steel and a method for pickling a corresponding metallic surface with reduced pickling removal, which or which completely with a subsequent Conversion treatment is compatible and toxicologically less harmful and less harmful to the environment.
  • the formation of the conversion coating are not adversely affected as well as a water-wettable surface are available.
  • the service life of a corresponding pickling bath should preferably be increased by the reduced pickling removal.
  • This object is achieved by a composition according to claim 1, a concentrate according to claim 7, a method according to claim 8 and a use according to claim 15.
  • Advantageous embodiments are each described in the dependent claims.
  • the aqueous composition according to the invention for reducing pickling during pickling of metallic surfaces containing bare and / or galvanized steel contains a mixture of a compound of the formula I.
  • an "aqueous composition” is to be understood to mean one which contains water, for the most part, ie more than 50% by weight, as the solvent / dispersant,
  • the aqueous composition is a solution, more preferably about a solution containing only water as a solvent.
  • the "galvanized steel” may in the present case be both electrolytically galvanized and hot-dip galvanized steel.
  • Compounds of Formula I act as physical corrosion inhibitors adsorbed to the metallic surface by van der Waals forces, forming a monomolecular, homogeneous, densely packed layer thereon. By means of said layer, the metallic surface is physically at least partially shielded from a proton attack and thus the pickling removal of the surface is prevented or at least reduced. It was surprisingly found that the use of certain mixtures of different compounds of the formula I, a significant synergy effect can be achieved with respect to a reduction of pickling.
  • the aqueous composition according to the invention is essentially free from ⁇ , ⁇ '-diethylthiourea, N, N'-di (o-tolyl) thiourea, ⁇ , ⁇ '-dibutylthiourea and hexamethylenetetraamine.
  • Substantially free means that the abovementioned compounds were not deliberately added to the composition, that is to say they are at most impurities in the starting materials used
  • the total content of these compounds in the composition according to the invention is preferably below 5 mg / l, more preferably below 1 mg / l.
  • The% by weight mixing ratio of the compound of formula I in which R 1 and R 2 are both H and the compound of formula I wherein R 1 and R 2 are each independently HO- (CH 2 ) W Group with w> 2 is preferably in the range of 0.5: 1 to 2: 1, more preferably in the range of 0.75: 1 to 1, 75: 1 and most preferably in the range 1: 1 to 1, 5: 1 (calculated as 2-butyne-1, 4-diol and 2-butyne-1, 4-diol-bis (2-hydroxyethyl ether)).
  • the sum of x and y is 2 to 5. More preferably, the aqueous composition contains a mixture of 2-butyne-1, 4-diol and 2-butyne-1, 4-diol bis (2-hydroxyethylether).
  • the mixing ratio based on% by weight is again preferably in the range from 0.5: 1 to 2: 1, more preferably in the range from 0.75: 1 to 1:75: 1 and most preferably in the range 1: 1 to 1, 5: 1.
  • the composition additionally contains at least one compound of formula II
  • the at least one compound of the formula II is preferably HO-CH 2 -S-CH 2 .
  • the aqueous composition according to the invention can be obtained from the concentrate according to the invention by dilution with a suitable solvent and / or dispersion medium, preferably with water, and optionally adjusting the pH.
  • the dilution factor when adding the concentrate to the pickling solution in step ii) is preferably in the range from 1:23 to 1: 225.
  • the dilution factor when adding the concentrate to the rinse solution in step iii) is preferably in the range from 1: 225 to 1: 2250.
  • the surface is formed in successive process steps i) optionally cleaned and / or rinsed,
  • iii) is brought into contact with an aqueous rinsing composition, wherein the pickling composition in step ii) and / or the rinsing composition in step iii) at least one composition according to the invention as described above.
  • the pickling composition ii) preferably contains at least one compound selected from the group consisting of phosphonates, condensed phosphates and citrate and / or at least one mineral acid selected from the group consisting of sulfuric acid, hydrochloric acid, hydrofluoric acid and nitric acid, more preferably it contains at least one mineral acid selected from the group consisting of sulfuric acid, hydrochloric acid, hydrofluoric acid and nitric acid, most preferably it contains sulfuric acid.
  • the pH of the rinsing composition in step iii) is preferably strongly acidic, neutral or slightly alkaline, more preferably in the range from 2 to 8.
  • the pickling composition in step ii) is a composition according to the invention as described above.
  • the total concentration of the mixture of the two compounds of the formula I in the mordant composition is preferably in the range from 31 to 620 mg / l, particularly preferably in the range from 31 to 310 mg / l (calculated as 2-butyne-1, 4-diol).
  • the use of the mixture of the two compounds of the formula I in the pickling composition has the advantage of particularly effectively reducing pickling.
  • the rinsing composition in step iii) is a composition according to the invention as described above.
  • the total concentration of the mixture of the two compounds of the formula I in the rinsing composition is preferably in the range from 3 to 62 mg / l, particularly preferably in the range from 3 to 31 mg / l (calculated as 2-butyne-1,4-diol).
  • the pickling composition in step ii) and the rinsing composition in step iii) are each a composition according to the invention as described above. In the mixing of the two compounds of the formula I in the pickling composition and in the rinsing composition may be the same or a different mixture.
  • the total concentration of the mixture of the two compounds of formula I in the pickling composition is again preferably in the range from 31 to 620 mg / l, more preferably in the range from 31 to 310 mg / l (calculated as 2-butyne-1, 4-diol ) and in the rinsing composition preferably in the range of 3 to 62 mg / l, more preferably in the range of 3 to 31 mg / l (calculated as 2-butyne-1, 4-diol).
  • metallic surface containing bare and / or galvanized steel to the surface of a metallic component / workpiece, such as a steel pipe, of wires or screws (general cargo).
  • the pickled with the inventive method metallic surface is therefore preferably used in the field of parts treatment.
  • the pickled and rinsed metallic surface is preferably first conversion treated.
  • For the conversion treatment is preferably a acid aqueous composition containing zinc phosphate, manganese phosphate and optionally nickel ions (so-called zinc phosphating).
  • an acidic aqueous composition which comprises a titanium, zirconium and / or hafnium compound and optionally copper ions and / or a compound which liberates copper ions, if appropriate a polymer and / or copolymer and, if appropriate, one Organoalkoxysilane and / or a hydrolysis and / or a condensation product thereof.
  • a base coat which is preferably a cathodic electrodeposition paint (KTL), more preferably a (meth) acrylate- or epoxy-based KTL, is applied, and then a top coat is applied.
  • KTL cathodic electrodeposition paint
  • a lubricant containing salts, polymers and / or soaps is applied to the pickled and rinsed metallic surface.
  • the present invention is to be illustrated by the following - not to be limited - embodiments.
  • Aqueous pickling solutions A to E were prepared, each containing 20% by weight of H 2 SO 4 , 50 g / L of Fe 2+ and optionally one or two pickling inhibitors.
  • Test panels of CRS cold rolled steel were each weighed before treatment with one of the pickling solutions.
  • pickling inhibitors of pickling solutions B and C thus each had an excellent inhibition of 96%.
  • the inhibition values of the individual inhibitors but-2-yn-1,4-diol (pickling solution D) and 2-butyne-1,4-diol bis (2-hydroxyethyl ether) (pickling solution E) remained significant at 85% and 92%, respectively behind it.
  • the inhibition value of the mixture according to the invention of the latter two pickling inhibitors was surprisingly high at 97% and even exceeded that of the abovementioned pickling inhibitors to be avoided.
  • the sheets were subsequently zinc-phosphated.
  • the pickling solutions B and F were added to the phosphating bath in increasing amounts.
  • the appearance of the metal sheets was evaluated.
  • the layer weights in g / m 2 calculated from P2O 5 were determined by means of RFA.
  • the mixture according to the invention not only reduces the pickling rate, but also leads to no disruption of film formation in a subsequent phosphating step, for example as a result of the carryover of the pickling solution.

Landscapes

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

Abstract

La présente invention concerne une composition aqueuse pour la réduction de l'enlèvement par décapage lors du décapage de surfaces métalliques contenant de l'acier nu et/ou galvanisé, qui contient un mélange d'un composé de formule I R1O-(CH2)x-CEC-(CH2)y-OR2 (I), dans laquelle R1 et R2 sont tous deux H, et d'un composé de formule I, dans laquelle R1 et R2 sont respectivement indépendamment l'un de l'autre un groupe HO-(CH2) W avec w > 2, x et y étant respectivement indépendamment l'un de l'autre un nombre de 1 à 4 pour chacun des deux composés de formule I. L'invention concerne également un procédé de décapage d'une surface métallique correspondante avec un enlèvement par décapage réduit.
EP17721118.2A 2016-04-29 2017-04-28 Composition permettant de réduire l'enlèvement par décapage lors du décapage de surfaces métalliques contenant de l'acier nu et/ou galvanisé Active EP3449040B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL17721118T PL3449040T3 (pl) 2016-04-29 2017-04-28 Kompozycja do zmniejszania ubytku wskutek trawienia podczas trawienia powierzchni metalowych zawierających stal niepowlekaną i/lub ocynkowaną

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102016207429 2016-04-29
PCT/EP2017/060227 WO2017186929A1 (fr) 2016-04-29 2017-04-28 Composition permettant de réduire l'enlèvement par décapage lors du décapage de surfaces métalliques contenant de l'acier nu et/ou galvanisé

Publications (2)

Publication Number Publication Date
EP3449040A1 true EP3449040A1 (fr) 2019-03-06
EP3449040B1 EP3449040B1 (fr) 2020-03-18

Family

ID=58668882

Family Applications (1)

Application Number Title Priority Date Filing Date
EP17721118.2A Active EP3449040B1 (fr) 2016-04-29 2017-04-28 Composition permettant de réduire l'enlèvement par décapage lors du décapage de surfaces métalliques contenant de l'acier nu et/ou galvanisé

Country Status (12)

Country Link
US (1) US11124884B2 (fr)
EP (1) EP3449040B1 (fr)
JP (1) JP6968825B2 (fr)
KR (1) KR102369545B1 (fr)
CN (1) CN109072454B (fr)
DE (1) DE102017207232A1 (fr)
ES (1) ES2795655T3 (fr)
MX (1) MX2018013233A (fr)
PL (1) PL3449040T3 (fr)
RU (1) RU2747720C2 (fr)
WO (1) WO2017186929A1 (fr)
ZA (1) ZA201807922B (fr)

Families Citing this family (3)

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MX2019006442A (es) * 2016-12-02 2019-08-21 Ecolab Usa Inc Inhibidores de corrosion de hemiacetal de tiol-formilo.
MX2020001345A (es) 2017-08-03 2020-03-12 Ecolab Usa Inc Aductos de tiol para inhibicion de corrosion.
KR102655537B1 (ko) 2017-12-12 2024-04-09 케메탈 게엠베하 빙정석을 함유하는 침착물을 제거하기 위한 무-붕산 조성물

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Also Published As

Publication number Publication date
JP2019515133A (ja) 2019-06-06
ES2795655T3 (es) 2020-11-24
US11124884B2 (en) 2021-09-21
CN109072454B (zh) 2021-03-05
BR112018071497A2 (pt) 2019-02-19
US20190112717A1 (en) 2019-04-18
EP3449040B1 (fr) 2020-03-18
ZA201807922B (en) 2020-02-26
MX2018013233A (es) 2019-02-13
DE102017207232A1 (de) 2017-11-02
KR102369545B1 (ko) 2022-03-03
RU2018140856A3 (fr) 2020-06-25
RU2747720C2 (ru) 2021-05-13
CN109072454A (zh) 2018-12-21
PL3449040T3 (pl) 2020-08-24
WO2017186929A1 (fr) 2017-11-02
JP6968825B2 (ja) 2021-11-17
KR20190003514A (ko) 2019-01-09
RU2018140856A (ru) 2020-05-29

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