EP3372660A1 - Lubrifiants haute température - Google Patents

Lubrifiants haute température Download PDF

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Publication number
EP3372660A1
EP3372660A1 EP18000076.2A EP18000076A EP3372660A1 EP 3372660 A1 EP3372660 A1 EP 3372660A1 EP 18000076 A EP18000076 A EP 18000076A EP 3372660 A1 EP3372660 A1 EP 3372660A1
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EP
European Patent Office
Prior art keywords
oil
group
temperature
mixture
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.)
Granted
Application number
EP18000076.2A
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German (de)
English (en)
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EP3372660B1 (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 PL18000076T priority Critical patent/PL3372660T3/pl
Publication of EP3372660A1 publication Critical patent/EP3372660A1/fr
Application granted granted Critical
Publication of EP3372660B1 publication Critical patent/EP3372660B1/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
    • 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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    • C10M109/00—Lubricating compositions characterised by the base-material being a compound of unknown or incompletely defined constitution
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    • C10M111/06—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 compound of the type covered by group C10M109/00
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    • 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, especially oils and fats based on an aromatic ester, such as a trimellitic acid ester and mixtures of various trimellitic acid esters, alkylaromatics, estolides and a fully hydrogenated or hydrogenated polyisobutylene or a mixture thereof, a thickener.
  • the invention further relates to the use of this high temperature grease for continuous use temperatures of up to 250 ° C.
  • the lubricants must fulfill a variety of other tasks: they must 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.
  • Synthetic esters are often used as base oils for high-temperature applications since 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 friction coefficients and high wear resistance. In order to ensure uniform lubrication even at high temperatures, a liquid lubricant film must remain between metal parts during the entire processing process. Therefore, the lubricant must evaporate only slightly at the maximum processing temperature, form little residue and form as few cracking residues as possible.
  • lubricants ensure that a separating, load-transmitting lubricating film is built up between sliding or rolling parts. This ensures that the metallic surfaces do not touch and thus 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 due to high speeds or foreign heating, very low temperatures, for example, in camps that operate in cold environments or that occur in aerospace applications. Likewise, the modern lubricants under so-called clean room conditions should be used to avoid the pollution of the room by the abrasion or the consumption of lubricants.
  • Lubricants are also subject to special requirements in the application to the effect that the running surfaces of the bearings are not attacked by low friction, run the storage surfaces quiet, and long running times are achieved without relubrication. Also, lubricants must withstand the effects of force such as centrifugal force, gravity and vibration.
  • the object of the present invention is to provide a high temperature oil and high temperature grease which meets the above requirements.
  • the Vercrackungs Wegwarnote formed should not lend, but be redissolvable by fresh fat.
  • the high-temperature lubricant should have a good hydrolytic stability, corrosion and wear resistant, as well as have a good oxidation resistance and adapted to the requirement good low temperature behavior. This is defined by the pour point for lubricating oils and by the flow pressure at low temperatures for lubricating greases.
  • the high-temperature grease should show good noise behavior, have long maturities and cause substantially no signs of wear of the devices.
  • the high-temperature oil according to the invention and the high-temperature fat according to the invention are distinguished by outstanding performance.
  • the high-temperature oil or high-temperature grease according to the invention exhibits high thermal stability combined with a long service life and good lubricating properties.
  • the high-temperature oil according to the invention comprises as ester compound an estolide or a mixture of different estolides or an aliphatically substituted naphthalene or a mixture of different aliphatically substituted naphthalenes.
  • estolides are ester compounds which are acid or enzymatically catalyzed from fatty acids, preferably oleic acid or dicarboxylic acids, or a mixture of both.
  • the acid function attacks the double bond of an adjacent oil fatty acid molecule, resulting in a higher molecular weight ester compound.
  • the terminal acid group is then usually esterified with an alcohol, preferably 2-ethyl-hexanol and then the remaining double bonds are hydrogenated or esterified with carboxylic acid, for example acetic acid.
  • alcohols such as isoamyl alcohol or Guebert alcohols are also conceivable for the esterification of the terminal acid group.
  • estolides can also be synthesized via a condensation of hydroxycarboxylic acids or a condensation of hydroxycarboxylic acids with fatty acids, for example oleic acid or stearic acid derivatives.
  • the chain length of the hydroxycarboxylic acids or unsaturated acids used can range from C 6 to C 54 .
  • the acids may contain other functional groups such as amines, ethers, sulfur-containing groups.
  • the high temperature oil of the invention may contain a second oil comprising an alkylaromatic.
  • an aromatic is used.
  • an aromatic means a monocyclic, bicyclic or tricyclic ring system having four to fifteen carbon atoms, the monocyclic ring system being aromatic or at least one of the rings being aromatic in a bi- or tricylic ring system.
  • Preference is given to using a bicyclic ring system which preferably has 10 carbon atoms.
  • the aromatic is substituted with one or more aliphatic substituents.
  • Particularly preferred is the aromatic having one to four aliphatic substituents and in particular having two or three aliphatic substituents substituted.
  • An alkyl group according to the invention is a saturated aliphatic hydrocarbon group having 1 to 30, preferably 3 to 20, more preferably 4 to 17 and especially 6 to 15 carbon atoms.
  • An alkyl group may be linear or branched and is optionally substituted with one or more of the abovementioned substituents.
  • the lubricating oil particularly preferably contains at least one aliphatically substituted naphthalene, in particular at least one alkyl-substituted naphthalene.
  • the naphthalene is substituted with one to four aliphatic substituents and in particular with two or three aliphatic substituents.
  • the viscosity, measured at 40 ° C, of the aliphatically substituted naphthalene is preferably 30 to 600 mm 2 / s, more preferably 30 to 300 m 2 / s.
  • the high temperature oil of the invention further comprises a polyisobutylene.
  • a polyisobutylene By suitable choice of the polyisobutylene, in particular with regard to the degree of hydrogenation and molecular weight, the properties of the oil according to the invention, for example its kinematic viscosity and, above all, its formation of residues, can be influenced in a desired manner.
  • the polyisobutylene can be used in hydrogenated or fully hydrogenated form, as well as a mixture of hydrogenated and fully hydrogenated polyisobutylene can be used. Fully hydrogenated polyisobutylenes are preferably used.
  • the Polyisobutylene is present in an amount of 6 to 45 wt .-% in the composition, preferably 10 to 45 wt .-%, in particular 15 to 45 wt .-% are used.
  • the high-temperature oil according to the invention further comprises from 0.1 to 10 wt .-%, additives which are used individually or in combination and from the group consisting of anti-corrosion additives, antioxidants, anti-wear additives, UV stabilizers, inorganic or organic solid lubricants selected.
  • the high-temperature fat of the present invention comprises as an ester compound a trimellitic acid ester or a mixture of various trimellitic acid esters, wherein the alcoholic group of the ester is a linear or branched alkyl group having 8 to 16 carbon atoms.
  • the properties of the lubricant for example the viscosity, the viscosity-temperature behavior, the oxidation resistance and residue behavior can be adjusted.
  • the high temperature grease of the invention may contain a second oil comprising an alkyl aromatic.
  • an aromatic is used.
  • an aromatic means a monocyclic, bicyclic or tricyclic ring system having four to fifteen carbon atoms, the monocyclic ring system being aromatic or at least one of the rings being aromatic in a bi- or tricylic ring system.
  • Preference is given to using a bicyclic ring system which preferably has 10 carbon atoms.
  • the aromatic is substituted with one or more aliphatic substituents.
  • the aromatic is particularly preferably substituted by one to four aliphatic substituents and in particular by two or three aliphatic substituents.
  • An alkyl group according to the invention is a saturated aliphatic hydrocarbon group having 1 to 30, preferably 3 to 20, more preferably 4 to 17 and especially 6 to 15 carbon atoms.
  • An alkyl group may be linear or branched and is optionally substituted with one or more of the abovementioned substituents.
  • the lubricating grease particularly preferably contains at least one aliphatically substituted naphthalene, in particular at least one alkyl-substituted naphthalene.
  • the naphthalene is substituted with one to four aliphatic substituents and in particular with two or three aliphatic substituents.
  • the viscosity, measured at 40 ° C, of the aliphatically substituted naphthalene is preferably 30 to 600 mm 2 / s, more preferably 30 to 300 m 2 / s.
  • estolides can also be used.
  • Preferred viscosities, measured at 40 ° C are between 30 and 500 mm 2 / sec. Viscosities of 30 to 140 mm 2 / sec are particularly preferred.
  • the high-temperature grease according to the invention further comprises a polyisobutylene.
  • a polyisobutylene By suitable choice of the polyisobutylene, in particular with regard to the degree of hydrogenation and molecular weight, the properties of the fat according to the invention, for example its kinematic viscosity, can be influenced in a desired manner.
  • the polyisobutylene can be used in hydrogenated or fully hydrogenated form, as well as a mixture of hydrogenated and fully hydrogenated polyisobutylene can be used. Fully hydrogenated polyisobutylenes are preferably used.
  • the polyisobutylene is in an amount of 6 to 45 wt .-% in the composition, preferably 10 to 45 wt .-%, in particular 15 to 45 wt .-% are used.
  • the polyisobutylene has a number average molecular weight of 115 to 10,000 g / mol, preferably from 160 to 5000 g / mol.
  • the high-temperature fat according to the invention further comprises from 0.1 to 10 wt .-%, additives which are used individually or in combination and from the group consisting of corrosion protection additives, antioxidants, anti-wear additives, UV stabilizers, inorganic or organic solid lubricants selected.
  • the high-temperature fat according to the invention also comprises a thickener.
  • 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 may be used singly 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 , wherein R is an aryl, alky
  • the additives mentioned below have particularly good physical and chemical properties:
  • the addition of antioxidants can reduce or even prevent the oxidation of the oil or fat according to the invention, in particular when it is used. Oxidation can lead to undesirable free radicals and, as a result, decomposition reactions of the high-temperature lubricant can occur.
  • the addition of antioxidants stabilizes the high temperature grease.
  • Antioxidants which are particularly suitable according to the invention are the following compounds: Styrenated diphenylamines, diaromatic amines, phenolic resins, thiophenol resins, phosphites, butylated hydroxytoluene, butylated hydroxyanisole, phenyl-alphanaphthylamine, phenyl-beta-naphthylamine, octylated / butylated diphenylamine, dialpha-tocopherol, di-tert-butyl-phenyl, benzenepropanoic acid, sulfur-containing phenolic compounds , Phenolic compounds and mixtures of these components.
  • the high temperature grease may contain corrosion inhibiting additives, metal deactivators or ion complexing agents.
  • corrosion inhibiting additives 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 Diisooctylester reacted with (C 11-14 ) alkylamines, mixture of phosphoric acid and mono- and Diisooctylester reacted with tert-alkylamine and primary (C 12-14 ) amines, dodecanoic acid, triphenyl phosphorothionate and amine phosphates.
  • 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.
  • 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®, FLUORO ® FG, SYNALOX® 40-D, ACHESON® FGA 1820 and ACHESON® FGA 1810.
  • the grease may include 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, graphites, graphene, nano-tubes, 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, graphites, graphene, nano-tubes, SiO 2 modifications or a mixture thereof.
  • the high temperature oil or fat according to the invention has up to a temperature of 250 ° C no or negligible decomposition phenomena. By this is meant that less than 10% of the lubricant decomposes.
  • the high-temperature oil or fat according to the invention may contain, as another 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 Contain 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 Contain copolymers.
  • the high temperature oil or fat according to the invention contains an estolide, preferably the main constituents of the estolide being obtained by chemical or enzymatic processes starting from native oils from the group of sunflower oil, rapeseed oil, castor oil, linseed oil, corn oil, diest oil, soybean oil, linseed oil , Peanut oil, "Lesqueralle” oil, palm oil, olive oil or mixtures of the aforementioned oils.
  • native oils from the group of sunflower oil, rapeseed oil, castor oil, linseed oil, corn oil, diest oil, soybean oil, linseed oil , Peanut oil, "Lesqueralle” oil, palm oil, olive oil or mixtures of the aforementioned oils.
  • the high-temperature oil or fat according to the invention due to its physical and chemical properties, is outstandingly suitable for use in chains, rolling and sliding bearings, in vehicle technology, conveyor technology, mechanical engineering, office technology and in industrial plants and machines. but also in the fields of home appliances and consumer electronics. Due to its good temperature resistance, it can also be used at high operating temperatures up to 260 ° C, preferably at temperatures of 150 to 250 ° C.
  • the invention further relates to a process for the preparation of the above-described High temperature oils or fats, in which the base oils and the additives are mixed together.
  • Estolides or aliphatically substituted naphthalenes are initially charged in a stirred kettle. At 100 ° C, the polyisobutylene and optionally a further oil is added with stirring. Subsequently, the mixture is stirred for 1 h to obtain a homogeneous mixture. The anti-wear agents and the antioxidant are added to the kettle at 60 ° C with stirring. After about 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 optionally a further oil and the thickener is added with stirring.
  • the thickener is formed by an in situ reaction of the reactants used in the base oil. Subsequently, the mixture is heated to 150 ° C to 210 ° C, stirred for several hours and cooled again. In the cooling process at about 60 ° C, the necessary anti-wear agents, antioxidants and corrosion inhibitors are added.
  • a homogeneous mixture of the fat is obtained by the final homogenization step on roller, colloid mill or Gaulin.
  • compositions of the high temperature fats are shown in Table 6. ⁇ u> Table 6 ⁇ / u> Type Li complex Li complex Li complex Di-Harnstof Di-urea Di-urea Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Trimellitic acid esters [% 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 [wt.%] 26 25 25 25 25 25 25 25 25 25 Additive package [wt.%] 4 1 4 1 1 1 Thickener concentration [% by weight] 10 10 15.0 8.8 8.8 8.8
  • Example 7 Example 8 Walpenentration after 60 DT [DIN ISO 2137] 284 283 278 232 232 300 Walpenentration after 100000 DT [DIN ISO 2137] 324 319 319 254 254 338 Dropping point [C °] [DIN ISO 2176] > 300 > 300 > 300 > 300 280 292 Flow pressure -20 ° C; [mbar] [DIN 51805] > 2000 275 284 575 525 ⁇ 1400 Flow pressure -30 ° C; [mbar] [DIN 51805] > 2000 425 675 ⁇ 1400 ⁇ 1400 ⁇ 1400 Oil loss 40 ° C / 168h; [Weight%] [DIN 51817] 3.80 3 1.70 1.2 0.10 5,60 Oil level 150 ° C / 30h; [Weight%] [FTMS 761 C] 7.4
  • the evaporation losses of the different fat samples at 150 ° C after 30 h are between 2% and 5%, which underlines the very good thermal stability of these fat concepts.
  • the oil separation has a decisive influence on the lubricating effect of a grease. It is important to ensure that on the one hand, the oil separation is not too high and the oil runs out of the warehouse and thus the Tribo system is no longer available and on the other hand no oil separation is 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 lubricating film can form in the camp.
  • the greases of the examples were subjected to a FE 9 rolling bearing test according to DIN 51 821 in which the service life of the greases investigated is determined and the upper service temperature of greases in roller bearings at medium speeds and average axial loads is determined.
  • Table 8 shows that the runtimes through the use of PIB in combination with various base oils have long run times and are thus suitable for high application temperatures in continuous operation.
  • the noise behavior of the various fat formulations is very positively influenced by the use of fully hydrogenated polyisobutylene. With the exception of example 6, good to very good noise properties can be achieved.
  • Example 3 The property of the fat of Example 3 using fully hydrogenated PIB was now compared to a fat (Comparative Example 3) containing a PIB which still had double bonds, that is, a non-fully hydrogenated PIB.
  • the other composition of the fat according to Comparative Example 3 corresponded to that of Example 3. ⁇ u> Table 10 ⁇ / u> Example 3projectsbeisp.
  • Example 3 grease exhibits a doubled run time in the FE9 test, has lower evaporation losses and significantly better noise performance.
  • Table 11 shows that there are significant differences in the use of fully hydrogenated and partially hydrogenated PIB.
  • the dissolution of the residue based on the partially hydrogenated PIV is no longer possible, while the oil with the fully hydrogenated PIB has very good Wiederananseigenschaften.

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DK3372660T3 (da) 2021-12-20
DE102014018718A1 (de) 2016-06-23
BR112017012528A2 (pt) 2018-03-13
WO2016096074A3 (fr) 2016-09-01
PL3372660T3 (pl) 2022-01-31
EP3372659B1 (fr) 2021-06-16
PL3372659T3 (pl) 2021-10-25
ES2893843T3 (es) 2022-02-10
CN107406791A (zh) 2017-11-28
HUE057256T2 (hu) 2022-05-28
SI3372659T1 (sl) 2021-08-31
US20170327760A1 (en) 2017-11-16
WO2016096074A2 (fr) 2016-06-23
KR20170085089A (ko) 2017-07-21
MX2021012796A (es) 2021-11-12
CN107406791B (zh) 2021-01-01
JP2017538838A (ja) 2017-12-28
EP3372660B1 (fr) 2021-09-22
KR102019083B1 (ko) 2019-11-04
EP3372659A1 (fr) 2018-09-12
MX2017007674A (es) 2018-01-23
EP3234079A2 (fr) 2017-10-25
JP6448801B2 (ja) 2019-01-09
EP3234079B1 (fr) 2021-07-07

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