EP3234079B1 - Lubrifiants haute température - Google Patents

Lubrifiants haute température Download PDF

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Publication number
EP3234079B1
EP3234079B1 EP15801328.4A EP15801328A EP3234079B1 EP 3234079 B1 EP3234079 B1 EP 3234079B1 EP 15801328 A EP15801328 A EP 15801328A EP 3234079 B1 EP3234079 B1 EP 3234079B1
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EP
European Patent Office
Prior art keywords
group
oil
temperature grease
temperature
hydrogenated
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.)
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Application number
EP15801328.4A
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German (de)
English (en)
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EP3234079A2 (fr
Inventor
Karl EGERSDÖRFER
Thomas Kilthau
Stefan Grundei
Stefan Seemeyer
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.)
Klueber Lubrication Muenchen GmbH and Co KG
Original Assignee
Klueber Lubrication Muenchen SE and Co KG
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Publication date
Application filed by Klueber Lubrication Muenchen SE and Co KG filed Critical Klueber Lubrication Muenchen SE and Co KG
Priority to EP18000075.4A priority Critical patent/EP3372659B1/fr
Priority to PL18000075T priority patent/PL3372659T3/pl
Priority to PL18000076T priority patent/PL3372660T3/pl
Priority to EP18000076.2A priority patent/EP3372660B1/fr
Priority to DK18000076.2T priority patent/DK3372660T3/da
Publication of EP3234079A2 publication Critical patent/EP3234079A2/fr
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Publication of EP3234079B1 publication Critical patent/EP3234079B1/fr
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M111/00—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
    • C10M111/04—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential at least one of them being a macromolecular organic compound
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/02—Well-defined hydrocarbons
    • C10M105/06—Well-defined hydrocarbons aromatic
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    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/32—Esters
    • C10M105/36—Esters of polycarboxylic acids
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    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/02—Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation
    • C10M107/08—Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation containing butene
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2060/00—Chemical after-treatment of the constituents of the lubricating composition
    • C10N2060/02—Reduction, e.g. hydrogenation

Definitions

  • the invention relates to high-temperature lubricants, in particular greases based on alkyl aromatics, a fully hydrogenated or hydrogenated polyisobutylene or a mixture thereof and a thickener.
  • the invention also relates to the use of this high-temperature grease for continuous use temperatures of up to 250 ° C.
  • the lubricants have to fulfill a large number of other tasks: They have to cool, reduce friction, wear and power transmission, protect against corrosion and at the same time have a sealing effect.
  • the high-temperature greases should be quiet.
  • lubricants are not suitable for high-temperature applications because they are destroyed at high temperatures, for example via oxidation and / or thermal decomposition reactions and polymerizations, and their lubricating properties are severely restricted. During decomposition reactions, the lubricant is split into low-molecular volatile components. Their evaporation leads to undesirable changes in viscosity, loss of oil and excessive vapor formation. From this results in a loss of lubricating effect. The lubricants also lose their lubricating effect through polymerization due to the formation of insoluble polymerization products.
  • Synthetic esters are often used as base oils for high-temperature applications because they have very good oxidative, hydrolytic and thermal stability.
  • the lubricants In order to meet the diverse requirements of high-temperature applications, the lubricants must have, among other things, high stability, low coefficients of friction and high wear resistance. In order to be able to guarantee uniform lubrication even at high temperatures, a liquid lubricating film must remain between metal parts during the entire processing process. For this reason, the lubricant must only evaporate a little at the maximum processing temperature, form few residues and form as few cracking residues as possible.
  • lubricants ensure that a separating, load-transferring lubricating film is built up between parts sliding or rolling on each other. This ensures that the metallic surfaces do not touch each other and therefore no wear occurs.
  • the lubricants must therefore meet high requirements. These include extreme operating conditions such as very high or very low speeds, high temperatures caused by high speeds or external heating, very low temperatures, for example with bearings that work in a cold environment or that are used in the air and Space travel occur. Modern lubricants should also be able to be used under so-called clean room conditions in order to avoid room pollution from abrasion or the consumption of lubricants.
  • Lubricants when using modern lubricants, it should be avoided that they evaporate and thus "clog", ie that they become solid after a short application and no longer show any lubricating effect. Special requirements are also placed on lubricants when they are used in such a way that the running surfaces of the bearings are not attacked by low friction, the bearing surfaces run quietly, and long running times are achieved without relubrication. Lubricants also have to withstand the effects of forces such as centrifugal force, gravity and vibrations.
  • a lubricating grease can stimulate vibrations in the rolling bearing when it participates in circulation (rolling over, flexing), which are "lubricant noises" in the medium 300 to 1,800 Hz and high 1,800 to 10,000 Hz frequency bands, compared to the bearing noise in the low frequency band at 50 to 300 Hz.
  • the lubricant noise is superimposed by the noise peaks that occur when hard particles roll over the rolling elements in the form of shock pulses on the bearing ring.
  • the evaluation of the noise behavior is based on the SKF BeQuiet + method.
  • a fats are known which are in gel form, which are difficult to produce in a homogeneous and stable form. These difficulties can be caused, for example, by the thickening agent used or the base oil.
  • a fat is provided that is homogeneous, stable and effective and that the desired properties are achieved by the fact that lesser amounts of thickening agents and other additives are present in the fat.
  • a hydrogenated polymer of butene or isobutylene with a relatively low molecular weight was used and a small amount of thickener in the form of Al complex soaps was used.
  • the object of the present invention is to provide a high-temperature grease which meets the above-mentioned requirements.
  • the lubricating grease should exhibit a good lubricating effect over a long period of time at a high temperature.
  • the cracking residues formed should not be laked up, but should be able to be dissolved again by fresh fat.
  • the high-temperature lubricant should have good hydrolytic stability, be corrosion- and wear-resistant, as well as good oxidation resistance and good low-temperature behavior adapted to the requirements. This is defined for lubricating oils by the pour point and for lubricating greases by the flow pressure at low temperatures.
  • the high-temperature grease should exhibit good noise behavior, have long running times and essentially cause no signs of wear on the devices.
  • the high-temperature grease according to the invention is distinguished by excellent performance.
  • the high-temperature grease according to the invention shows high thermal stability combined with a long service life and good lubricating properties.
  • the viscosity, measured at 40 ° C., of the aliphatic substituted naphthalene is preferably from 30 to 600 mm 2 / s, more preferably from 30 to 300 m 2 / s.
  • the high temperature grease according to the invention can contain a second oil which comprises an alkyl aromatic.
  • An aromatic is preferably used.
  • an aromatic is understood to mean a monocyclic, bicyclic or tricyclic ring system with four to fifteen carbon atoms, the monocyclic ring system being aromatic or at least one of the rings in a bicyclic or tricyclic ring system being aromatic.
  • a bicyclic ring system which preferably has 10 carbon atoms, is preferably used.
  • the aromatic is preferably substituted by one or more aliphatic substituents.
  • the aromatic is particularly preferably substituted with one to four aliphatic substituents and in particular with two or three aliphatic substituents.
  • an alkyl group is a saturated aliphatic hydrocarbon group having 1 to 30, preferably 3 to 20, more preferably 4 to 17 and in particular 6 to 15 carbon atoms.
  • An alkyl group can be linear or branched and is optionally substituted with one or more of the above-mentioned substituents.
  • the lubricating grease particularly preferably contains at least one aliphatically substituted naphthalene, in particular at least one alkyl-substituted naphthalene.
  • the naphthalene is preferably substituted with one to four aliphatic substituents and in particular with two or three aliphatic substituents.
  • the viscosity, measured at 40 ° C., of the aliphatic substituted naphthalene is preferably from 30 to 600 mm 2 / s, more preferably from 30 to 300 m 2 / s.
  • the high-temperature grease according to the invention further comprises a polyisobutylene.
  • the polyisobutylene can be used in hydrogenated or fully hydrogenated form, and a mixture of hydrogenated and fully hydrogenated polyisobutylene can also be used. Fully hydrogenated polyisobutylenes are preferably used.
  • the polyisobutylene is present in the composition in an amount of 6 to 45 percent by weight, preferably 10 to 45 percent % By weight, in particular 15 to 45% by weight, are used.
  • the polyisobutylene has a number average molecular weight of 115 to 10,000 g / mol, preferably 160 to 5000 g / mol.
  • the high-temperature grease according to the invention also comprises from 0.1 to 10% by weight, additives, which are used individually or in combination and are selected from the group consisting of corrosion protection additives, antioxidants, wear protection additives, UV stabilizers, inorganic or organic solid lubricants.
  • the high-temperature grease according to the invention also comprises a thickening agent.
  • the thickener in the high-temperature grease of the lubricant composition according to the invention is either a reaction product of a diisocyanate, preferably 2,4-diisocyanatotoluene, 2,6-diisocyanatotoluene, 4,4'-diisocyanatodiphenylmethane, 2,4'-diisocyanatophenylmethane, 4,4'-diisocyanatodi- phenyl, 4,4'-diisocyanato-3-3'-dimethylphenyl, 4,4'-diisocyanato-3,3'-dimethylphenylmethane, which can be used individually or in combination, with an amine of the general formula R ' 2 -NR , or a diamine of the general formula R ' 2 -NR-NR' 2 , where R is an aryl, alky
  • additives for high-temperature oils and greases the following additives have particularly good physical and chemical properties:
  • antioxidants can reduce or even prevent the oxidation of the oil or fat according to the invention, especially when it is used. In the event of oxidation, undesirable free radicals can arise and, as a result, more decomposition reactions of the high-temperature lubricant occur.
  • the high temperature fat is stabilized by adding antioxidants.
  • Antioxidants particularly suitable according to the invention are the following compounds: Styrenated diphenylamines, diaromatic amines, phenolic resins, thiophenolic resins, phosphites, butylated hydroxytoluene, butylated hydroxyanisole, phenyl-alphanaphthylamine, phenyl-beta-naphthylamine, octylated / butylated diphenylamine, dialpha-tocopherol, phenyl-phenyl-phenol, sulfur-propane, phenyl-tert-butyl-phenyl compounds , Phenolic compounds and mixtures of these components.
  • the high-temperature grease can also contain corrosion protection additives, metal deactivators or ion complexing agents. These include triazoles, imidazolines, N-methylglycine (sarcosine), benzotriazole derivatives, N, N-bis (2-ethylhexyl) -ar-methyl-1H-benzotriazole-1-methanamine; n-Methyl-N (1-oxo-9-octadecenyl) glycine, mixture of phosphoric acid and mono- and diisooctyl esters reacted with (C 11-14 ) -alkylamines, mixture of phosphoric acid and mono- and diisooctyl esters reacted with tert-alkylamine and primary (C 12-14 ) amines, dodecanoic acid, triphenyl phosphorothionate and amine phosphates.
  • metal deactivators or ion complexing agents include triazoles, imidazolines,
  • IRGAMET® 39 IRGACOR® DSS G, amine O; SARKOSYL® O (Ciba), COBRATEC® 122, CUVAN® 303, VANLUBE® 9123, CI-426, CI-426EP, CI-429 and CI-498.
  • anti-wear additives are amines, amine phosphates, phosphates, thiophosphates, phosphorothionates and mixtures of these components.
  • the commercially available anti-wear additives include IRGALUBE® TPPT, IRGALUBE® 232, IRGALUBE® 349, IRGALUBE® 211 and ADDITIN® RC3760 Liq 3960, FIRC-SHUN® FG 1505 and FG 1506, NA-LUBE® KR-015FG, LUBEBOND .®, FLUORBOND ® FG, SYNALOX® 40-D, ACHESON® FGA 1820 and ACHESON® FGA 1810.
  • the grease can contain solid lubricants such as PTFE, BN, pyrophosphate, Zn oxide, Mg oxide, pyrophosphates, thiosulfates, Mg carbonate, Ca carbonate, Ca stearate, Zn sulfide, Mo sulfide, W sulfide, Sn -Sulfide, graphite, graphene, nanotubes, SiO 2 modifications or a mixture thereof.
  • solid lubricants such as PTFE, BN, pyrophosphate, Zn oxide, Mg oxide, pyrophosphates, thiosulfates, Mg carbonate, Ca carbonate, Ca stearate, Zn sulfide, Mo sulfide, W sulfide, Sn -Sulfide, graphite, graphene, nanotubes, SiO 2 modifications or a mixture thereof.
  • the high-temperature grease according to the invention can contain, as a further base oil, an oil, preferably selected from the group consisting of mineral oil, aliphatic carboxylic acid and dicarboxylic acid esters, fatty acid triglycerides, pyromellitic acid esters, diphenyl ethers, phloroglucinic esters and / or poly-alpha-olefins, alpha-olefin copolymers.
  • an oil preferably selected from the group consisting of mineral oil, aliphatic carboxylic acid and dicarboxylic acid esters, fatty acid triglycerides, pyromellitic acid esters, diphenyl ethers, phloroglucinic esters and / or poly-alpha-olefins, alpha-olefin copolymers.
  • the high-temperature grease according to the invention due to its physical and chemical properties, is excellent for use in chains, roller and plain bearings, in vehicle technology, conveyor technology, mechanical engineering, office technology and in industrial systems and machines, but also in the Areas of household machines and consumer electronics. Due to its good temperature resistance, it can also be used at high operating temperatures of up to 260 ° C, preferably at temperatures of 150 to 250 ° C.
  • the invention also relates to a method for producing the above-described high-temperature grease, in which the base oils and the additives are mixed with one another.
  • Estolides or aliphatically substituted naphthalenes are placed in a stirred tank. At 100 ° C., the polyisobutylene and, if necessary, a further oil are added with stirring. Then the mixture is stirred for 1 hour to obtain a homogeneous mixture. The anti-wear agents and the antioxidant are added to the kettle at 60 ° C. while stirring. After approx. 1 hour, the finished oil can be filled into the containers provided.
  • the base oil is placed in a stirred tank. At 100 ° C., the polyisobutylene and, if necessary, a further oil and the thickener are added with stirring. The thickener results from an in situ reaction of the reactants used in the base oil. The mixture is then heated to 150 ° C. to 210 ° C., stirred for several hours and cooled again. In the cooling process at approx. 60 ° C, the necessary wear protection agents, antioxidants and corrosion protection agents are added. A homogeneous mixture of the fat is obtained by the final homogenization step using a roller, colloid mill or the Gaulin.
  • compositions of the high temperature greases are shown in Table 6. ⁇ u> Table 6 ⁇ /u> Type Li complex Li complex Li complex Di-urea Di-urea Di-urea Reference example 3
  • Example 7 Reference example 8 Trimellitic acid ester [% by weight] 60 0 0 65.2 0 0 Estolide [wt.%] 0 0 56 0 0 65.2 alkylated naphthalene [wt.%] 0 64 0 0 65.2 0 fully hydrogenated polyisobutylene [% by weight] 26th 25th 25th 25th 25th 25th 25th Additive package [wt.%] 4th 1 4th 1 1 1 Thickener concentration [wt.%] 10 10 15.0 8.8 8.8 8.8
  • the thickeners used in Examples 3 to 8 are: Reference example 3: LiOH, 12-hydroxystearic acid, azelaic acid, Example 4: LiOH, 12-hydroxystearic acid, azelaic acid, Reference example 5: LiOH, 12-hydroxystearic acid, azelaic acid, Reference example 6: Di-urea; Methylene-diphenyl-diisocyanate (MDI), octylamine, oleylamine Example 7: Di-urea; MDI, octylamine, oleylamine Reference example 8: Di-urea; MDI, octylamine, oleylamine
  • Oil separation has a decisive influence on the lubricating effect of a grease. It must be ensured that, on the one hand, the oil separation is not too high and the oil runs out of the bearing and is therefore no longer available to the tribo-system and, on the other hand, no oil separation can be observed and the lubricating effect of the grease is lost.
  • the oil separation should ideally be between 0.5 and 8 wt .-%, so that an optimal Can form a lubricating film in the bearing.
  • the greases in the examples were subjected to an FE 9 roller bearing test according to DIN 51 821, in which the service life of the greases examined is determined and the upper service temperature of lubricating greases in roller bearings at medium speeds and medium axial loads is determined.
  • Table 8 shows that the running times due to the use of PIB in conjunction with various base oils have long running times and are therefore suitable for high application temperatures in continuous operation.
  • Table 11 shows that there are significant differences when using fully hydrogenated and partially hydrogenated PIB. For example, it is no longer possible to partially dissolve the residue on the basis of the partially hydrogenated PIB, while the oil with the fully hydrogenated PIB has very good redissolving properties.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Lubricants (AREA)

Claims (5)

  1. Graisse haute température comprenant
    a) 91,9 à 25% en poids d'une huile au moins sélectionnée parmi le groupe des alkylaromatiques,
    b) 6 à 45% en poids d'un polymère sélectionné parmi le groupe constitué d'un polyisobutylène hydrogéné ou intégralement hydrogéné ou d'un mélange de polyisobutylènes hydrogénés ou intégralement hydrogénés,
    c) 0,1 à 10% en poids d'additifs individuellement ou en combinaison, sélectionnés parmi le groupe constitué d'additifs anti-corrosion, d'antioxydants, d'additifs anti-usure, de stabilisateurs UV, de lubrifiants solides anorganiques ou organiques, et
    d) 2 à 20% en poids d'un épaississant.
  2. Graisse haute température suivant la revendication 1, dont le composant huileux comprend comme huile supplémentaire un composé sélectionné parmi le groupe constitué d'huile minérale, d'esters d'acide carboxylique et d'acide dicarboxylique aliphatiques, de triglycérides d'acides gras, d'ester d'acide pyromellitique, de diphényléther, d'ester de phloroglucine et/ou de poly-alpha-oléfines, de copolymères d'alpha-oléfines.
  3. Graisse haute température suivant la revendication 1, dont l'épaississant est sélectionné parmi le groupe constitué d'urée, de savons complexes d'aluminium, de savons simples métalliques des éléments du premier et second groupe principal de la classification périodique, de savons complexes métalliques des éléments du premier et second groupe principal de la classification périodique, de bentonites, de sulfonates, de silicates, d'aérosil, de polyimides, de PTFE ou d'un mélange des épaississants mentionnés ci-avant.
  4. Graisse haute température suivant la revendication 1, dont le composé alkylaromatique est un naphtalène substitué par un aliphatique.
  5. Utilisation de la graisse haute température suivant une des revendications précédentes pour le graissage de roulements et de paliers lisses, dans les domaines de la technique automobile, de la technique de transport, de la construction de machines, de la technique bureautique ainsi que des machines et installations industrielles, mais encore dans les domaines des appareils domestiques, de l'électronique grand public et pour le graissage de chaînes, de poulies de chaînes et de bandes de presses continues.
EP15801328.4A 2014-12-17 2015-11-19 Lubrifiants haute température Active EP3234079B1 (fr)

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PL18000076T PL3372660T3 (pl) 2014-12-17 2015-11-19 Wysokotemperaturowe środki smarowe
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DE102014018718A1 (de) 2016-06-23
MX2017007674A (es) 2018-01-23
JP2017538838A (ja) 2017-12-28
BR112017012528A2 (pt) 2018-03-13
PL3372660T3 (pl) 2022-01-31
SI3372659T1 (sl) 2021-08-31
EP3372660A1 (fr) 2018-09-12
KR20170085089A (ko) 2017-07-21
PL3372659T3 (pl) 2021-10-25
EP3372659B1 (fr) 2021-06-16
WO2016096074A2 (fr) 2016-06-23
JP6448801B2 (ja) 2019-01-09
KR102019083B1 (ko) 2019-11-04
EP3372660B1 (fr) 2021-09-22
HUE057256T2 (hu) 2022-05-28
CN107406791B (zh) 2021-01-01
ES2893843T3 (es) 2022-02-10
EP3372659A1 (fr) 2018-09-12
CN107406791A (zh) 2017-11-28
MX2021012796A (es) 2021-11-12
WO2016096074A3 (fr) 2016-09-01
EP3234079A2 (fr) 2017-10-25
DK3372660T3 (da) 2021-12-20

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