WO2017029287A1 - Schmierfettzusammensetzungen - Google Patents

Schmierfettzusammensetzungen Download PDF

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Publication number
WO2017029287A1
WO2017029287A1 PCT/EP2016/069423 EP2016069423W WO2017029287A1 WO 2017029287 A1 WO2017029287 A1 WO 2017029287A1 EP 2016069423 W EP2016069423 W EP 2016069423W WO 2017029287 A1 WO2017029287 A1 WO 2017029287A1
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WO
WIPO (PCT)
Prior art keywords
grease composition
composition according
weight
boron nitride
binder
Prior art date
Application number
PCT/EP2016/069423
Other languages
German (de)
English (en)
French (fr)
Inventor
Rachel Kling
Alexander GRECHIN
Bernard FISIC
Karl-Heinz Hensel
Original Assignee
Setral Chemie 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 Setral Chemie Gmbh filed Critical Setral Chemie Gmbh
Priority to EP16754263.8A priority Critical patent/EP3337879B1/de
Priority to CN201680047719.8A priority patent/CN108026465A/zh
Priority to US15/753,786 priority patent/US20180245010A1/en
Priority to ES16754263T priority patent/ES2902836T3/es
Publication of WO2017029287A1 publication Critical patent/WO2017029287A1/de
Priority to HK18116649.1A priority patent/HK1257564A1/zh

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    • 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
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/50—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing halogen
    • C10M105/54—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing halogen containing carbon, hydrogen, halogen and oxygen
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M113/00—Lubricating compositions characterised by the thickening agent being an inorganic material
    • C10M113/10—Clays; Micas
    • C—CHEMISTRY; METALLURGY
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    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/26—Compounds containing silicon or boron, e.g. silica, sand
    • C—CHEMISTRY; METALLURGY
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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
    • C10M169/02—Mixtures of base-materials and thickeners
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
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    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • C10M2201/0416—Carbon; Graphite; Carbon black used as thickening agents
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
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    • C10M2201/061—Carbides; Hydrides; Nitrides
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    • C10M2201/0626—Oxides; Hydroxides; Carbonates or bicarbonates used as thickening agents
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    • C10M2201/0656—Sulfides; Selenides; Tellurides used as thickening agents
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    • C10M2201/085—Phosphorus oxides, acids or salts
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    • C10M2201/085—Phosphorus oxides, acids or salts
    • C10M2201/0856—Phosphorus oxides, acids or salts used as thickening agent
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    • C10M2201/087—Boron oxides, acids or salts
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    • C10M2201/087—Boron oxides, acids or salts
    • C10M2201/0876—Boron oxides, acids or salts used as thickening agent
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10—Compounds containing silicon
    • C10M2201/102—Silicates
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    • C10M2201/1026—Silicates used as thickening agents
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    • C10M2201/1056—Silica used as thickening agents
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    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/1033—Polyethers, i.e. containing di- or higher polyoxyalkylene groups used as base material
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    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/04—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen
    • C10M2213/043—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen used as base material
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    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/06—Perfluoro polymers
    • C10M2213/0606—Perfluoro polymers used as base material
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    • C10M2213/06—Perfluoro polymers
    • C10M2213/062—Polytetrafluoroethylene [PTFE]
    • C10M2213/0623—Polytetrafluoroethylene [PTFE] used as base material
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    • C10M2213/062—Polytetrafluoroethylene [PTFE]
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    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
    • C10M2229/051—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing halogen
    • C10M2229/0515—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing halogen used as base material
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    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy

Definitions

  • the present invention relates to lubricating grease compositions which are particularly suitable as high-temperature lubricating greases and for lubrication in kiln systems,
  • Greases generally contain a thickener dissolved or dispersed in a base oil, often with dispersants for better and more stable distribution of the thickener.
  • the thickener is used to adjust the desired consistency, with a variety of inorganic and organic
  • the base oils are mineral oils and synthetic oils. Frequently, perfluorinated polyalkyl ethers (PFPE), i. fluorinated synthetic oils with good lubricating properties that are chemically non-reactive, high temperature stable and therefore non-toxic (see, e.g.
  • PFPE perfluorinated polyalkyl ethers
  • WO 97/47710 describes lubricating grease compositions containing as a base oil a mixture of a hydrocarbon oil and a perfluorinated one
  • Polyalkyletheröl PFPE
  • a thiourea-based thickener PFPE
  • the composition may also include polytetrafluoroethylene (PTFE) and conventional additives.
  • PTFE polytetrafluoroethylene
  • EP 657 524 describes lubricating grease compositions comprising a hydrogenated base mineral oil and / or a synthetic oil, a perfluorinated polyalkyl ether oil and a
  • Thickener PTFE included.
  • Thickening agent in particular a polyurea, and a distributed in the grease inorganic material such as silica.
  • WO 2008/154997 A1 describes a grease containing a base oil, an ionic liquid, a thickener and an additive.
  • the ionic liquid should cause an increase in the life and lubricity of the lubricant and serve to adjust the viscosity and the electrical conductivity.
  • Lubricants such as polyfluorinated compounds, to the limits of Material resilience and are therefore no longer applicable in spite of excellent sliding and lubricating properties in the higher temperature range.
  • WO 2013/037456 therefore describes high-temperature fats which contain a fluorine-free base oil, a thickener which may be PTFE, additives and optionally a further fluorine-free oil component.
  • EP 1589291 A1 discloses a furnace exhaust guide having rolling elements arranged in a rolling element cage.
  • Molybdenum sulfide Molybdenum sulfide, tungsten disulfide or boron nitride, and which is applied and baked in the form of a paint
  • WO 2010/046456 A1 describes a pullout guide for an oven, in which the tracks of the pullout guide are lubricated with boron nitride and / or a lubricant containing polysiloxane.
  • EP 648 832 A1 describes lubricating grease compositions which are fluorinated
  • Polymer oil Polymer oil, boron nitride and optionally solid fluorinated polymers.
  • Grease compositions are said to have good lubricating properties even under harsh operating conditions.
  • Perfluoropolyether oil having a kinematic viscosity of 50-1500 mm 2 / s at 40 ° C, optionally contain a thickener and other conventional additives.
  • Grease compositions are also believed to be useful in contact with graphite or molybdenum disulfide at higher temperatures.
  • PTFE-containing greases form toxic fumes at higher temperatures and are also relatively quickly washed out during cleaning operations by water.
  • PTFE-free greases in turn have the disadvantage that they are washed out even faster by water than PTFE-containing greases.
  • the object of the present invention is therefore to provide lubricating grease compositions with improved water washability.
  • the lubricating grease compositions are said to have improved temperature stability and to provide a longer lubricating life at high temperatures.
  • This object is achieved by a grease composition comprising at least one high-viscosity, fluorinated oil, hexagonal boron nitride and a binder.
  • the present invention therefore relates to a grease composition comprising
  • the kinematic viscosity is measured with SVM 300 Viscometer, Anton Paar at a temperature of 40 ° C.
  • component (a) comprises fluorinated, in particular perfluorinated, polyalkyl ether oils or fluorinated silicone oils, in particular perfluorinated silicone oils, and
  • Suitable perfluorinated polyalkyl ether oils are described, for example, in WO 97/47710 or EP 657 524, to which reference is made in its entirety.
  • the perfluorinated polyalkyl ether oils correspond to the formula:
  • a 1 is -CF 3 , -C 2 F 5 , or -C 3 F 7 ;
  • a 2 is -OCF 3 , -OC 2 F 5 , or -OC 3 F 7 ; a, b, c, d, e and f are statistically distributed and are 0 or an integer from 1 to 200, wherein not all of them can simultaneously stand for 0.
  • e / a and f / a are in the range of 20 to 50 and b / a in the range of 0.5 to 2.
  • c and d are 0.
  • Particularly preferred are the perfluorinated polyalkyl ethers of the following units:
  • perfluorinated polyalkyletherols correspond to the formula:
  • a, e and f are randomly distributed and represent 0 or an integer of 1 to 200, not all of which can simultaneously stand for 0 and e / a and f / a are in the range of 20 to 50.
  • the perfluorinated polyalkyletherols correspond to the formula:
  • A - (X) a -O-A '- (X') b - where A 'is a perfluoropolyether chain containing one or more of (CF 2 O),
  • X and X ' are the same or different and are -CF 2 -, -CF 2 CF 2 - or
  • a and b are the same or different and stand for integers having a value of 0 or 1, with the proviso that in the case of the block A bound to the end group TO, the subscript a stands for 1 and in which the end group T ' bound block A, the index b is 0;
  • B is a block of units derived from one or more olefins of the formula (Ia) of which at least one is free-radically homopolymerizable
  • j is an integer from 1 to 5
  • j ' is an integer from 0 to 4, with the proviso that (j + j') is greater than 2 and less than 5;
  • Ri, R2, RSS, R 4, R E, R 6, R 7 and R 8 are identical or different and are selected from halogen; H; CrC 6 - (per) haloalkyl, wherein the halogen is F and / or Cl; C 1 -C 6 -alkyl optionally containing heteroatoms; and CrC 6 -oxy (per) fluoroalkyl are selected;
  • z is an integer greater than or equal to 2;
  • B ' is a block which is derived from one or more olefins of the formula (Ia), but where at least one of the substituents R 1 to R 8 is different than in block B, where (j + j') is greater than or equal to 2 and less than 5;
  • component (a) may additionally comprise a non-fluorinated oil, in particular a mineral oil.
  • the non-fluorinated oil is generally contained in an amount of 0.1 to 40% by weight, more preferably 0.5 to 30% by weight, based on the amount of the fluorinated oil.
  • the grease composition further comprises boron nitride, especially hexagonal boron nitride.
  • the grease composition comprises hexagonal ⁇ -boron nitride.
  • the boron nitride has a BET surface area in the range of 10 to 20 m 2 / g, determined according to ISO 9277: 2010.
  • the boron nitride has an average particle size D50 of 1 to 10 ⁇ m, in particular 2 to 6 ⁇ m, determined by means of laser diffractometry (Malvern Mastersizer 3000).
  • a suitable boron nitride for example, under the trade name BORONID ® from ESK Ceramics GmbH & Co. KG, Germany, available.
  • the grease composition further comprises a binder.
  • the binder generally has an average particle size D50 in the range of 1 to 10 ⁇ m, preferably 2 to 8 ⁇ m, determined by means of laser diffractometry.
  • the binder is selected from bentonite,
  • Particularly preferred is the binder organically modified bentonite or a mixture of organically modified bentonite with at least one further binder selected from alkali metal phosphates, aluminum phosphates, alkali metal silicates, alkaline earth metal silicates, aluminum silicates, alkaline earth metal carbonates, silica, titania, alumina and mixtures thereof.
  • the further binder is generally contained in an amount of 0.1 to 50 wt .-%, in particular 0.5 to 40 wt .-%, based on the amount of organically modified bentonite.
  • silica organically modified fumed silica is preferable, and as the titania, organic-modified fumed titania is preferable.
  • Modified fumed silica and modified fumed titanium dioxide are products that have been surface-treated with an organosilane, especially with an alkylsilane.
  • Corresponding products such as Aerosil R 912, Aerosil 812, Aerosil 805, Aerosil R 202, Aeroxide ® Ti0 2 T 805, Aeroxide ® Ti0 2 NKT 90, VP NKT 65 are commercially available, for example from Evonik Industries AG, Germany or Wacker Chemie AG, Germany.
  • Bentonite is a mixture of different clay minerals with the most important
  • montmorillonite (60% to 80%). Further accompanying minerals are quartz, mica, feldspar, pyrite or calcite.
  • quartz, mica, feldspar, pyrite or calcite The term "bentonite” includes all of course
  • Bentonite is commercially available in the form of various commercial products.
  • Organic hydrophobically modified bentonite can, for example, by the reaction of natural or purified bentonite with quaternary ammonium compounds in the sense of a cation exchange reaction in which, for example, alkali cations against quaternary Ammonium compounds are exchanged done.
  • Quaternary ammonium compounds suitable for this reaction are, for example, those of the general formula R 1 R 2 R 3 R 4 N + X " , where X is one equivalent of an anion, for example sulfate, hydrogensulfate, alkylsulfate, arylsulfate, alkylsulfonate, arylsulfonate, halide, phosphate , carbonate, alkyl phosphate, alkyl carbonate, nitrate, alkoxide, hydroxide, tetrafluoroborate or perchlorate, in particular halide, and R 1, R 2, R 3 or R 4 may be the same or different and may stand for -C 2 o alkyl.
  • X is one equivalent of an anion, for example sulfate, hydrogensulfate, alkylsulfate, arylsulfate, alkylsulfonate, arylsulfonate, halide, phosphate ,
  • R 1 and R 2 identical or different, represent -C 4 alkyl and R 3 and R 4, identical or different, are 2 -C 2 o-alkyl is Ci.
  • quaternary ammonium salts can be used, where X is halide, in particular chloride, R 1 and R 2 are methyl and R 3 and R 4, identical or different, are C 6 -C 8 -alkyl BARAGEL ⁇
  • the commercial product is bentonite modified with Me 2 N (Ci. 6 - Ci 8 alkyl) 2 CI.
  • the lubricating grease composition additionally comprises water in an amount of 0.01 to 1% by weight, in particular 0.05 to 0.2% by weight, based on the total mass of the composition.
  • Water serves as an activating agent for bentonite, in particular for activating the dispersing and thickening properties of the bentonite.
  • the lubricating grease composition according to the invention may contain at least one additive, in particular an additive which is customary in the field of lubricating grease compositions.
  • the additive is selected from antioxidants, for example, functionalized perfluoropolyalkyl ethers as described in EP 1 354 932 A1 and US 5,550,277; Wear protection additives, for example functionalized perfluoropolyalkyl ethers, as described in WO 2016/020232;
  • Corrosion inhibitors for example sodium sebacate, functionalized perfluoropolyalkyl ethers as described in US 5,550,277; Dyes, for example azo dyes and solid lubricants, for example molybdenum disulfide, tungsten disulfide, tin sulfide.
  • inventive compositions for example sodium sebacate, functionalized perfluoropolyalkyl ethers as described in US 5,550,277
  • Dyes for example azo dyes and solid lubricants, for example molybdenum disulfide, tungsten disulfide, tin sulfide.
  • the inventive composition each based on the total weight of the composition. According to a further embodiment, the inventive composition
  • Grease composition (a) 50-96% by weight of at least one perfluorinated polyalkyl ether oil
  • the lubricant composition is substantially free of PTFE.
  • the grease composition is substantially free of an ionic liquid.
  • the grease composition is substantially free of graphite.
  • “Substantially free” means that the lubricating grease composition contains less than 0.5% by weight of PTFE, less than 0.5% by weight of ionic liquid or less than 0.5% by weight of graphite, in particular each 0% by weight. % of these components, based on the
  • Grease compositions have a number of advantageous properties compared to known greases: very good compatibility of all components,
  • the lubricating grease compositions according to the invention are for lubrication in
  • applications include the lubrication of: Rolling and plain bearings, sliding guides, valves, joints, slides, column guides, ejectors and other sliding surfaces such as in
  • Circular conveyors paint lines, calenders, kiln cars, fans, switches,
  • Film stretching plants extraction plants, textile machines, wood press systems, pumps, dryers, motors, tire molds, construction machines, electrical and automotive engineering,
  • Paper industry and steel industry and machinery and equipment e.g. in the food and feed industry.
  • the grease composition according to the invention for the lubrication of sliding guides and wheels in kiln systems or rolling and sliding bearings in
  • the application of the grease composition is carried out by applying to the parts to be lubricated in a suitable amount for lubrication.
  • the grease composition of the invention is applied as a paste.
  • the grease composition can be easily applied be without the grease composition, for example, at the ends of the tracks of Ofenauszugsschienen run out or drip.
  • Optional post-treatment after application of the lubricating grease composition by vibratory grinding allows better distribution and adhesion of the grease on, for example, a metallic substrate.
  • the lubricant composition is thixotropic, i. upon mechanical action the viscosity decreases and the original viscosity returns after the end of the shear stress. This allows the pastes to be relatively easily spread on the surface of, for example, oven tray rails under pressure loading without dripping.
  • BARAGEL® (14.9 wt%, organic hydrophobically modified bentonite from Elementis Specialties Inc., USA) was added to the mixing kettle, the heater was turned off, and the resulting mixture was stirred for five minutes. Then, 0.1% by weight of water was added and the mixture was stirred for 30 minutes. After cooling to room temperature, boron nitride (5% by weight Boronid®, ESK Ceramics GmbH & Co. KG, Germany) and a corrosion inhibitor (2% by weight, Irgacor®, BASF SE, Germany) were added to the mixing vessel and the resulting Mixture was stirred for 30 min. The resulting BARAGEL® (14.9 wt%, organic hydrophobically modified bentonite from Elementis Specialties Inc., USA) was added to the mixing kettle, the heater was turned off, and the resulting mixture was stirred for five minutes. Then, 0.1% by weight of water was added and the mixture was stirred for 30 minutes. After cooling to room temperature, boron nitride
  • Grease was homogenized with a roller mill.
  • the data in% by weight are each based on the total weight of the grease.
  • the grease composition prepared according to Example 1 was first subjected to a VKA test (four-ball apparatus, ASTM D1831 / DIN 51350-4).
  • the VKA welding force became 4800 N and the VKA wear 0.9 mm at 150 kg / 1 min
  • Comparative samples (Comparative Example 1, Comparative Example 2, Comparative Example 3) were carried out washability tests. For this, the various samples were on
  • Example 1 weight loss after the third wash: ⁇ 50%; Rail is easy to move.
  • the PTFE-containing Comparative Example 2 develops toxic, vaporous
  • Comparative samples (Comparative Examples 4 and 5) were run endurance tests. For this purpose, the various samples were applied to furnace extension rails and the pull-out rails mounted on side rails. Then the grids were installed in an oven. A test load was placed in the middle of a baking tray in the oven. The entry and exit of the weighted baking sheet was carried out using a
  • Pneumatic cylinder performed.
  • the rails were subjected to an endurance test with 24000 cycles. After every 6000 cycles, motive force and lowering of the rails were checked, and also after every 6000 cycles, the rails were subjected to a dishwasher washing cycle. After a total of 24,000 cycles was the
  • composition of the comparative examples (wt .-%, based on the total weight of
  • Example 1 The sample passed the test (5 washes, good
  • Comparative Example 5 The sample failed the test (failed after 12,000 cycles, balls stuck for lack of greasing).

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Lubricants (AREA)
PCT/EP2016/069423 2015-08-20 2016-08-16 Schmierfettzusammensetzungen WO2017029287A1 (de)

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CN201680047719.8A CN108026465A (zh) 2015-08-20 2016-08-16 润滑脂组合物
US15/753,786 US20180245010A1 (en) 2015-08-20 2016-08-16 Lubricating grease composition
ES16754263T ES2902836T3 (es) 2015-08-20 2016-08-16 Composiciones de grasa lubricante
HK18116649.1A HK1257564A1 (zh) 2015-08-20 2018-12-27 潤滑脂組合物

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CN112646636A (zh) * 2020-12-22 2021-04-13 刘超 一种润滑油添加剂及其制备方法
AU2019258487B2 (en) * 2018-04-26 2021-10-21 Shell Internationale Research Maatschappij B.V. Lubricant composition and use of the same as a pipe dope

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CN111996064A (zh) * 2020-09-23 2020-11-27 上海虎头化工有限公司 一种超高温润滑脂及其制备方法

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EP0648832A1 (en) * 1993-09-13 1995-04-19 Dow Corning Corporation Grease compositions employing fluorinated polymer oils and hexagonal lattice boron nitride
WO1997047710A1 (de) * 1996-06-07 1997-12-18 KLüBER LUBRICATION MüNCHEN KG Schmierfettzusammensetzungen
US20080167208A1 (en) * 2005-02-22 2008-07-10 Miyuki Hashida Lubricant

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JP4926411B2 (ja) * 2005-04-08 2012-05-09 出光興産株式会社 グリース組成物
DE112009000197B4 (de) * 2008-02-01 2015-07-16 Nok Klueber Co. Ltd. Verwendung einer fluorhaltigen Diamid-Verbindung

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EP0648832A1 (en) * 1993-09-13 1995-04-19 Dow Corning Corporation Grease compositions employing fluorinated polymer oils and hexagonal lattice boron nitride
WO1997047710A1 (de) * 1996-06-07 1997-12-18 KLüBER LUBRICATION MüNCHEN KG Schmierfettzusammensetzungen
US20080167208A1 (en) * 2005-02-22 2008-07-10 Miyuki Hashida Lubricant

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2019258487B2 (en) * 2018-04-26 2021-10-21 Shell Internationale Research Maatschappij B.V. Lubricant composition and use of the same as a pipe dope
US11591539B2 (en) 2018-04-26 2023-02-28 Shell Usa, Inc. Lubricant composition and use of the same as a pipe dope
CN112646636A (zh) * 2020-12-22 2021-04-13 刘超 一种润滑油添加剂及其制备方法

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EP3337879B1 (de) 2021-11-17
ES2902836T3 (es) 2022-03-30

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