CN115461434A - 锂复合杂化润滑脂 - Google Patents
锂复合杂化润滑脂 Download PDFInfo
- Publication number
- CN115461434A CN115461434A CN202180034746.2A CN202180034746A CN115461434A CN 115461434 A CN115461434 A CN 115461434A CN 202180034746 A CN202180034746 A CN 202180034746A CN 115461434 A CN115461434 A CN 115461434A
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- CN
- China
- Prior art keywords
- weight
- grease
- lithium
- esters
- bearings
- 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
Links
- 239000004519 grease Substances 0.000 title claims abstract description 98
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 61
- 230000001050 lubricating effect Effects 0.000 title claims description 14
- 239000002131 composite material Substances 0.000 title claims description 9
- 239000000203 mixture Substances 0.000 claims description 86
- 150000002148 esters Chemical class 0.000 claims description 52
- 239000010702 perfluoropolyether Substances 0.000 claims description 49
- 239000000314 lubricant Substances 0.000 claims description 45
- 239000003921 oil Substances 0.000 claims description 44
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 23
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 23
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- 125000004432 carbon atom Chemical group C* 0.000 claims description 14
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- 238000000034 method Methods 0.000 claims description 13
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- 229920006007 hydrogenated polyisobutylene Polymers 0.000 claims description 12
- 125000003545 alkoxy group Chemical group 0.000 claims description 10
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical class C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 10
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
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- 150000001555 benzenes Chemical class 0.000 claims description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
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- 150000004696 coordination complex Chemical class 0.000 claims description 2
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- 125000002444 phloroglucinyl group Chemical class [H]OC1=C([H])C(O[H])=C(*)C(O[H])=C1[H] 0.000 claims description 2
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- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical compound [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 claims description 2
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 235000014692 zinc oxide Nutrition 0.000 claims description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 2
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- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 6
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- 238000011065 in-situ storage Methods 0.000 description 4
- 238000009434 installation Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- FSYKKLYZXJSNPZ-UHFFFAOYSA-N sarcosine Chemical compound C[NH2+]CC([O-])=O FSYKKLYZXJSNPZ-UHFFFAOYSA-N 0.000 description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
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- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 description 3
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 2
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 2
- 108010077895 Sarcosine Proteins 0.000 description 2
- 150000003973 alkyl amines Chemical class 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
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- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 2
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical class OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 2
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- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 2
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- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical class OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 2
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- DIOYAVUHUXAUPX-ZHACJKMWSA-N 2-[methyl-[(e)-octadec-9-enoyl]amino]acetic acid Chemical compound CCCCCCCC\C=C\CCCCCCCC(=O)N(C)CC(O)=O DIOYAVUHUXAUPX-ZHACJKMWSA-N 0.000 description 1
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Images
Classifications
-
- 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
- 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
-
- 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
- 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
- C10M105/18—Ethers, e.g. epoxides
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Abstract
本发明涉及提供基于与PFPE润滑脂组合的锂复合润滑脂的新型锂复合杂化润滑脂,其可在高温下使用,在此不形成漆膜并表现出低硬化倾向。本发明进一步涉及所述新型锂复合杂化润滑脂在车辆领域和工业领域中的部件中的用途。
Description
本发明涉及提供基于与PFPE润滑脂组合的锂复合润滑脂的新型锂复合杂化润滑脂,其可在高温下使用,在此不形成漆膜并表现出低硬化倾向。本发明进一步涉及所述新型锂复合杂化润滑脂在车辆领域中的部件中的用途。
杂化润滑脂是由至少两种彼此不混溶的基础油组成的混合物。例如,含有作为增稠剂的脲或脲/PTFE混合物和酯/PFPE作为不混溶基础油组分的杂化润滑脂代表这些润滑脂的一个重要类别。这些润滑脂使得有可能封闭在大约180℃(如在无氟润滑脂中实现)至270℃(这有可能用纯PTPE/PFPE润滑脂实现)之间的温度间隙。这些产品也比纯PFPE/PTFE润滑脂更容易适应特定要求。这是因为对于PFPE油,只有很少已知的可溶性添加剂,以致例如PFPE油的抗腐蚀性质只能在有限程度上得到改进。因此在PFPE/PTFE润滑脂中使用固体物质如亚硝酸钠或氧化镁作为抗腐蚀剂。但是,确保固体在部件表面上的均匀分布比用含有溶解的抗腐蚀添加剂的油润湿部件表面难得多。因此,包含于非含氟液相中的杂化润滑脂的添加剂能够比纯PFPE/PTFE润滑脂更好地实现如抗腐蚀性之类的性质。杂化润滑脂中的PFPE油含量的降低和杂化润滑脂的较低密度另外带来显著的成本优势。例如EP0902828B1中描述的酯/PFPE/PTFE/脲润滑脂或如例如US 6,063,743中描述的酯/PTFE/脲润滑脂的缺点在于,这些润滑脂在高温下具有后硬化的倾向并具有非常低的油分离。此外,当用于特定弹性体时,它们在一些情况下可能受到批评,以致它们不能用于广泛范围,例如滚柱轴承、瓦楞纸板装置。此外,氟化润滑脂非常昂贵,因此也需要在生产上具有成本效益并具有与氟化润滑脂相同或甚至更好的性质的杂化润滑脂。
与酯/脲润滑脂相比,锂复合润滑脂具有较高的油分离和在高温下较低的硬化倾向。但是,上限使用温度明显低于脲杂化润滑脂,这通常与过高的油分离有关或可归因于使用具有较低耐热性的基础油,如聚α烯烃或矿物油。
因此本发明的目的是提供克服上述缺点并表现出相应足够的油分离和即使在高温下也低的硬化的锂复合杂化润滑脂。
通过将含有聚异丁烯和酯的锂复合润滑脂与PFPE油或PFPE润滑脂,特别是PFPE/PTFE润滑脂组合并因此有可能实现与酯/脲/PFPE杂化润滑脂匹配的高温性能而没有表现出其缺点,令人惊讶地实现这一目的。通过这两种润滑脂的用量比例的选择,可以令人惊讶地调节油分离以使油分离低于用于混合的这两种润滑脂。
本发明进一步提供将部件,特别是在车辆技术中的滚动轴承、滑动轴承、传递和正时链中的部件润滑或上油的方法,其包括施加根据本发明的润滑剂组合物。
还提供将连铸装置中的滑轮轴承、连续加热炉中的输送滚柱轴承、回转炉、管式磨、转鼓和混合器中的开放齿圈、瓦楞纸板装置或膜拉伸装置中的轴承、用于生产和运输食品的装置中的轴承润滑或上油的方法,其包括施加根据本发明的润滑剂组合物。
根据本发明的润滑剂组合物包含
(A) 酯或酯混合物,其特别是选自偏苯三酸酯、均苯四酸酯、二聚酸酯、交内酯(Estolide),
(B) 聚异丁烯,
(C) 锂复合皂和
(D) PFPE油。
优选的根据本发明的润滑剂组合物包含
(A) 酯或酯混合物,其特别是选自偏苯三酸酯、均苯四酸酯、二聚酸酯、交内酯,
(B) 聚异丁烯,
(C) 锂复合皂,
(D) PFPE油和
(E) 附加增稠剂。
特别优选的根据本发明的润滑剂组合物包含
(A) 酯或酯混合物,其特别是选自偏苯三酸酯、均苯四酸酯、二聚酸酯、交内酯,
(B) 聚异丁烯,
(C) 锂复合皂,
(D) PFPE油和
(E) PTFE作为附加增稠剂。
尤其优选的根据本发明的润滑剂组合物包含
(A) 酯或酯混合物,其特别是选自偏苯三酸酯、均苯四酸酯、二聚酸酯、交内酯,
(B) 聚异丁烯,
(C) 锂复合皂,
(D) PFPE油和
(F) 附加基础油,其中烷基化二苯醚是优选的。
另一优选的根据本发明的润滑剂组合物包含
(A) 酯或酯混合物,其特别是选自偏苯三酸酯、均苯四酸酯、二聚酸酯、交内酯,
(B) 聚异丁烯,
(C) 锂复合皂,
(D) PFPE油和
(E) 附加增稠剂和
(F) 烷基化二苯醚。
根据本发明的润滑剂可含有(G)添加剂和(H)固体润滑剂作为附加组分。
组分(A)
组分(A)以70重量%至7重量%,优选60重量%至15重量%的量包含于根据本发明的润滑剂组合物中。
组分(A)是酯或酯混合物,其中该酯选自偏苯三酸酯(其包含作为烷氧基的含有6至18个碳原子,优选8至14个碳原子的直链或支化烷基,其中烷氧基可以相同或不同)、均苯四酸酯(优选四(2-乙基己基)均苯四酸酯)、氢化或未氢化的二聚酸酯(优选双(2-乙基己基)二聚酸酯)、交内酯。
交内酯应理解为是指含有由羟基羧酸,例如12-羟基硬脂酸或不饱和羧酸,例如油酸的均聚物构成的低聚单元的酯。合适的交内酯描述在例如US 6,018,063、US 6,316,649、WO 2018/177588 A1和US 2013/0261325 A1中。
组分(B)
组分(B)是聚异丁烯或聚丁烯并以0.5重量%至20重量%的量包含于根据本发明的组合物中;优选使用1.5重量%至15重量%。
组分(B)是如例如Synthetics, Mineral Oils and Bio Based LubricantsChemistry and Technology, 第二版, 编辑Leslie R. Rudnik, 作者M. Casserino, J.Corthouts, CRC Press 2013, 第273 - 300页, (ISBN 978-1-4398-5537-9)中描述的聚合物。
聚异丁烯的合适选择(特别是在氢化程度和分子量方面)能够以所需方式影响根据本发明的润滑脂的性质,例如其动态粘度。聚异丁烯可以以非氢化、氢化或完全氢化的形式使用,同样可使用非氢化、氢化和完全氢化的聚异丁烯的混合物。优选使用完全氢化的聚异丁烯。非氢化聚异丁烯由于其生产而含有不饱和端基。氢化或部分氢化的聚异丁烯应理解为是指其溴值比具有相同数均分子质量的未氢化聚异丁烯低至少20%的聚合物。因此,对于Mn为1300 g/mol的非氢化聚异丁烯,溴值为14克溴/100克聚异丁烯。完全氢化的聚异丁烯的溴值低于7克溴/100克聚异丁烯。溴值根据ASTM D2170-09(2018年重新批准)测定。
在另一个优选的实施方案中,聚异丁烯具有115至10000 g/mol,优选500至5000g/mol的数均分子量。通过根据ISO 16014-1,2019-05版的凝胶渗透色谱法测定数均分子量。
组分(C)
组分(C)以1重量%至18重量%,优选4重量%至14重量%的量包含于根据本发明的润滑剂组合物中。
组分(C)是锂复合皂。锂复合皂应理解为是指单官能羧酸,优选具有8至22个碳原子的羧酸,尤其优选具有14至20个碳原子的羧酸,尤其优选12-羟基硬脂酸和/或硬脂酸的锂盐与更高官能羧酸,优选具有6至14个碳原子的二羧酸,尤其优选壬二酸、癸二酸和十二烷二酸的锂盐的混合物。锂复合皂可另外含有短链羧酸,如乙酸和乳酸和/或膦酸和/或硼酸作为附加酸组分。
组分(D)
组分(D)是根据式(I)的全氟聚醚(PFPE):
其中R1和R2相同或不同并选自-CF3、-C2F5或C3F7,v、w、x、y、z是≥ 0至500的整数。
PFPE油例如以品牌名Aflunox®、Krytox®、Fomblin®和Demnum®销售。
PFPE油以5重量%至70重量%,优选15重量%至50重量%的量包含于根据本发明的润滑剂组合物中。
组分(E)
根据本发明的锂复合杂化润滑脂可包含除锂复合增稠剂外的附加增稠剂(E)。
附加增稠剂(E)以1重量%至30重量%,优选3重量%至20重量%的量包含于根据本发明的润滑剂组合物中。
根据本发明的杂化润滑脂中的附加增稠剂(E)选自Al复合皂、不含锂的周期表第一和第二主族元素的金属单皂(Einfachseife)、不含锂的周期表第一和第二主族元素的金属复合皂、膨润土、磺酸盐、硅酸盐、气相二氧化硅(Aerosil)、聚酰亚胺或PTFE或上述增稠剂的混合物。特别优选的附加增稠剂是PTFE。优选的PTFE以微粉形式使用,其由高分子量PTFE通过加热或通过辐射以实现分子量降解而制成。
组分(F)
根据本发明的杂化润滑脂可含有以0重量%至20重量%,优选2重量%至20重量%的量包含于根据本发明的润滑剂组合物中的附加油(F)。
组分(F)选自矿物油、烷基化苯、烷基化萘、脂族羧酸酯和二羧酸酯、脂肪酸甘油三酯、烷基化二苯醚、间苯三酚酯、交内酯和/或聚α-烯烃、α-烯烃共聚物、茂金属催化的聚α-烯烃。优选的附加油是烷基化二苯醚油。烷基化二苯醚油例如由Moresco公司以商品名Hilube®销售。该烷基含有10至20个碳原子。平均1至3个烷基键合到二苯醚基本单元。
组分(G)
根据本发明的润滑剂组合物进一步包含0重量%至10重量%,优选0.1重量%至10重量%的单独或组合使用的添加剂(G)。
组分(G)选自抗腐蚀添加剂、抗氧化剂、抗磨添加剂、紫外线稳定剂。既可以使用可溶于组分(A)的添加剂,又可以使用可溶于组分(D)的PFPE油的添加剂,或也可以使用不溶于这两种油相的添加剂。
抗氧化剂的实例是苯乙烯化二苯胺、二芳基胺、酚树脂、苯硫酚树脂、亚磷酸酯、丁基化羟基甲苯、丁基化羟基苯甲醚、苯基-α-萘胺、苯基-β-萘胺、辛基化/丁基化二苯胺、二-α-生育酚、二叔丁基酚或二叔丁基-4-甲基酚、苯丙酸、含硫的酚化合物、酚化合物和这些组分的混合物。
合适的抗腐蚀添加剂的实例包括金属减活剂或离子络合剂。这些包括三唑、咪唑啉、N-甲基甘氨酸(肌氨酸)、苯并三唑衍生物、N,N-二(2-乙基己基)-芳-甲基-1H-苯并三唑-1-甲胺;n-甲基-N(1-氧代-9-十八烯基)甘氨酸、磷酸和单-和二异辛酯与(C11-14)-烷基胺反应的混合物、磷酸和单-和二异辛酯与叔烷基胺和伯(C12-14)-胺反应的混合物、十二烷酸、硫代磷酸三苯酯和磷酸胺。市售添加剂是以下:IRGAMET® 39、IRGACOR® DSS G、Amin O;SARKOSYL® O (Ciba)、COBRATEC® 122、CUVAN® 303、VANLUBE® 9123、CI-426、CI-426EP、CI-429和CI-498。
附加抗磨添加剂是胺、磷酸胺、磷酸酯、硫代磷酸酯和这些组分的混合物。所列举的化合物通常包含有机基团。市售抗磨添加剂包括IRGALUBE® TPPT、IRGALUBE® 232、IRGALUBE® 349、IRGALUBE® 211和ADDITIN® RC3760 Liq 3960、FIRC-SHUN® FG 1505和FG1506、NA-LUBE® KR-015FG、LUBEBOND®、FLUORO® FG、SYNALOX® 40-D、ACHESON® FGA 1820和ACHESON® FGA 1810。
还可以包含PFPE衍生物作为添加剂。例如PFPE羧酸、其金属盐和铵盐、其酯和酰胺衍生物。进一步合适的物质描述在例如WO01/72759A1、WO 01/27916A1、EP1070074B1、EP1659165B1和US2015011446A1中。
组分(H)
根据本发明的润滑剂组合物可进一步含有固体润滑剂(H),其选自BN、焦磷酸盐、氧化锌、氧化镁、焦磷酸盐、硫代硫酸盐、碳酸镁、碳酸钙、硬脂酸钙、硫化锌、硫化钼、硫化钨、硫化锡、石墨、石墨烯、纳米管、SiO2变型或其混合物。固体润滑剂(H)以0重量%至10重量%,优选2重量%至5重量%的量包含于根据本发明的润滑剂组合物中。
根据本发明的润滑剂组合物用于部件的领域,特别是车辆技术、轨道车辆、输送技术、膜拉伸装置、瓦楞纸板装置中的滚动轴承、滑动轴承、传递和正时链,滑轮轴承、风扇轴承、牵引发动机的轴承的领域、用于润滑锥齿轮和正齿轮传动装置、弹簧、螺杆和压缩机、气动组件、阀和机器部件以及在偶尔无意与食品发生接触的装置中。
附图显示根据本发明的锂杂化复合润滑脂的优点。
图1显示工作后针入度(Walkpenetration)60 dT,
图2显示油分离,即来自润滑脂的油损失。
现在参考以下实施例更详细阐释本发明。
根据本发明的润滑剂组合物的生产
根据本发明的润滑剂组合物的生产不受限制并可通过所有合适的方法进行。
根据本发明的润滑剂组合物的生产可以例如通过用组分(A)和/或(B)和/或(F)生产基础油混合物来进行。将锂复合增稠剂(C)所需的酸熔融到全部或仅部分预先装载在含有加热、冷却和搅拌单元的合适反应容器中的这种基础油混合物中,并加入氢氧化锂水溶液。这形成含有羧酸的锂皂的料液。可以逐一加入酸并中和,或首先加入单羧酸并中和并在第二步骤中加入更高官能羧酸并中和。将该料液加热到130℃以逐出水。通过在150℃至210℃下的热处理进行增稠剂(锂复合皂)的溶胀。然后将热处理过的料液冷却,其中也可使用一部分基础油混合物。组分(D)、(E)、(G)、(H)和任选未用于基础油混合物的组分(A)、(B)和(F)在合适的温度下添加并通过搅拌进行预均质化。
可溶于基础油混合物的固体润滑剂添加剂例如在高于其熔点的温度下添加。液体添加剂或非熔融添加剂/固体润滑剂/增稠剂组分在低于80℃的温度下添加。所得锂复合杂化润滑脂可通过合适的装置,如三辊磨、胶体磨或Gaulin均质机进行均质化。
上述方法在一个过程中制成根据本发明的润滑剂组合物。或者,在上述方法中可以省略PFPE油(D)和任选增稠剂组分(E)的添加以形成锂复合润滑脂。可以通过如上所述的搅拌、均质化来合并组分(D)和(E)以提供PFPE润滑脂。锂复合润滑脂和PFPE润滑脂可在第二方法步骤中合并以由其通过搅拌和均质化制成根据本发明的润滑剂组合物。
也可通过连续方法进行生产,其中也可使用粉末形式的现成Li复合皂。
实施例1
几种根据本发明的润滑剂组合物的生产、与用于生产的锂复合润滑脂和PFPE/PTFE润滑脂的比较、与脲杂化润滑脂的比较
生产
分开生产锂复合皂润滑脂(润滑脂A)和PFPE/PTFE润滑脂(润滑脂B),这两种润滑脂A和B以不同比率混合、搅拌并用辊均质化。
润滑脂A
作为基础油,生产由77%的来自烷基二苯醚(100 mm2/sec/40℃)和偏苯三酸酯和完全氢化的聚异丁烯(完全氢化,Mn大约1300 g/mol)的混合物组成的锂复合润滑脂,其中建立100 mm2/sec的在40℃下的粘度,然后加入15%的来自壬二酸和12-羟基硬脂酸的锂复合物和8%的由胺类抗氧化剂、磷酸酯、噻二唑、三唑和磷酸胺组成的添加剂套装。工作后针入度为270 1/10 mm(见表1)。
润滑脂B
生产含有70%的来自直链和支化PFPE的混合物(在40℃下的动态粘度200 mm2/sec)、26%的PTFE微粉(平均粒度d50(激光衍射,DIN ISO 9277)大约5 µm、比表面积(DINISO 9277)大约5 m2/g)和4%的作为抗腐蚀添加剂的癸二酸二钠的PFPE/PTFE 润滑脂。工作后针入度为286 1/10 mm(见表1)。
实施例1 (B1)
润滑脂A和润滑脂B在10重量%比90重量%的比率下的混合物。
实施例2 (B2)
润滑脂A和润滑脂B在30重量%比70重量%的比率下的混合物。
实施例3 (B3)
润滑脂A和润滑脂B在50重量%比50重量%的比率下的混合物。
实施例4 (B4)
润滑脂A和润滑脂B在70重量%比30重量%的比率下的混合物。
实施例5 (B5)
润滑脂A和润滑脂B在90重量%比10重量%的比率下的混合物。
对比例1 (VG1)
生产由50重量%的润滑脂B和50重量%的脲润滑脂组成的脲杂化润滑脂。该脲润滑脂由偏苯三酸酯和作为脲增稠剂的辛胺/油胺与MDI/TDI混合物的反应产物以及添加剂的混合物组成。基础油粘度为大约80 mm2/sec。工作后针入度为265 mm2/sec(见表2)。
对比例2 (VG2)
生产由基于二聚酸的复合酯(在40℃下的V 40为大约400 mm2/sec)和具有大约400 mm2/sec的动态粘度的支化PFPE油以2:1的质量比组成的脲杂化润滑脂。脲增稠剂以10%的比例包含,并且是辛胺/油胺与MDI/TDI混合物的反应产物。还包含8重量%的PTFE粉末(如润滑脂B中)和5重量%的可溶性添加剂(抗氧化剂、磷酸胺)。工作后针入度为290 mm2/sec(见表2)。
表1显示实施例B1至B5的根据本发明的锂复合杂化润滑脂以及润滑脂A和B的一般特征值。
表1
参数/润滑脂 | 润滑脂(B) | B1 | B2 | B3 | B4 | B5 | 润滑脂(A) |
工作后针入度60 dT [1/10 mm] (DIN ISO 2137) | 286 | 279 | 254 | 253 | 262 | 273 | 270 |
100000 dT后的Δ工作后针入度[1/10 mm] (DIN ISO 2137) | 15 | 28 | 31 | 45 | 44 | 39 | 45 |
滴点[℃] (DIN ISO 2176) | >300 | >300 | >300 | >300 | >300 | 294 | >300 |
流动压力[毫巴] (-40℃) (DIN 51805) | 200 | 375 | 575 | 850 | 875 | 875 | 925 |
流动压力[毫巴] (-50℃) (DIN 51805) | 325 | 575 | 1025 | >1400 | >1400 | >1400 | >1400 |
在25℃、剪切速率300 1/s下的剪切粘度(DIN 53019-1, -3) | 6095 | 7557 | 7253 | 7210 | 6849 | 6106 | 5966 |
蒸发损失,22h/100℃ [重量%] (DIN 58397) | 0.12 | 0.19 | 0.24 | 0.36 | 0.36 | 0.45 | 0.46 |
油分离,24h/150℃ [重量%] (ASTM D 6184) | 6.93 | 7.42 | 2.05 | 0.57 | 1.49 | 3.95 | 5.18 |
油分离,72h/150℃ [重量%] (ASTM D 6184) | 7.24 | 7.75 | 2.81 | 0.73 | 3.01 | 7.12 | 7.84 |
油分离,168h/40℃ [重量%] (DIN 51817) | 2.88 | 2.89 | 1.28 | 0.22 | 0.76 | 1.29 | 1.41 |
耐水性,静态,3h/90℃ (DIN 51807) | 0 | 0 | 1 | 1 | 1 | 1 | 1 |
铜腐蚀,24h/120℃ (DIN 51811) | 2 | 1-2 | 1 | 1 | 1 | 1 | 1 |
表2显示对比例VG1至2的数据。
表2
参数/润滑脂 | VG1 | VG2 |
工作后针入度60 dT [1/10 mm] (DIN ISO 2137) | 262 | 290 |
100000 dT后的Δ工作后针入度[1/10 mm] (DIN ISO 2137) | 47 | 43 |
滴点[℃] (DIN ISO 2176) | 285 | 285 |
流动压力[毫巴] (-40℃) (DIN 51805) | 725 | 625 |
流动压力[毫巴] (-50℃) (DIN 51805) | 1200 | 1375 |
在25℃、剪切速率300 1/s下的剪切粘度(DIN 53019-1, -3) | 5913 | 11880 |
蒸发损失,22h/100℃ [重量%] (DIN 58397) | 0.37 | 0.42 |
油分离,24h/150℃ [重量%] (ASTM D 6184) | 0.42 | 0.11 |
油分离,72h/150℃ [重量%] (ASTM D 6184) | 0.52 | 0.21 |
油分离,168h/40℃ [重量%] (DIN 51817) | 0.82 | 0.39 |
耐水性,静态,3h/90℃ (DIN 51807) | 0 | 0 |
铜腐蚀,24h/120℃ (DIN 51811) | 1 | 1 |
如图1(根据本发明的组合物的工作后针入度)中显而易见,组合物B2、B3和B4尤其表现出比两种使用的润滑脂A和B低的工作后针入度。这显示由这两种润滑脂类型组合得到根据本发明的组合物而带来的出乎意料的协同效应。
如图2(根据本发明的组合物的油分离的比较)中显而易见,根据本发明的组合物所显示的油分离比用于制造它们的润滑脂A和B低。这一行为显示由根据本发明的组合物带来的出乎意料的协同效应。油分离几乎达到两种对比产品VG1和VG2的低值。与对比润滑脂B相比的油分离的降低证明优于纯PFPE/PTFE润滑脂的优点。
数据还表明,通过润滑脂A和B的量的选择,可以设定所需油分离行为。
蒸发损失的测定
测试根据本发明的润滑剂组合物的热耐受性并将结果尤其与脲杂化润滑脂的热耐受性进行比较。为此进行关于称入不锈钢皿的5克初始重量的润滑脂在200℃下的蒸发和热应力下粘度的研究。结果显示在表3和4中。
根据DIN标准58397测定蒸发损失。对于各润滑脂样品,需要各三个不锈钢制蒸发损失皿。皿的几何参数描述在用于测定蒸发损失的标准(DIN 58397)中。最初测定皿的各自空重量。随后在三个蒸发损失皿中填充润滑脂样品。在此必须注意的是润滑脂的施加避免气泡。使用刮板修平表面并除去已进入皿的边缘凹部的过量润滑脂。随后将皿储存在具有对流的常规实验室干燥箱中,其中门关闭并且在相应的试验温度(在此为200℃)下。在每种情况下预定的持续时间(48 h、96 h、144 h和168 h)后,将皿从干燥箱中取出并使其冷却。然后将皿称重。由初始重量与测量重量之差测定蒸发损失。使用三个单独值测定平均值(VM)。与三个初始重量的平均值(AM)一起,可以计算蒸发损失。V = (VM/AM)*100[%]。在称重后,将皿置于干燥箱中,直至下一时间点。重复这一操作,直至已经过168小时。
表3
蒸发损失试验200℃ | B1 | B2 | B3 | B4 | B5 | ||
蒸发损失试验48h/200℃ | DIN 58397 | 重量% | 3.97 | 6.60 | 11.28 | 14.51 | 16.44 |
蒸发损失试验96h/200℃ | DIN 58397 | 重量% | 5.27 | 8.75 | 15.22 | 19.69 | 22.17 |
蒸发损失试验144h/200℃ | DIN 58397 | 重量% | 6.33 | 10.63 | 18.42 | 24.71 | 27.91 |
蒸发损失试验168h/200℃ | DIN 58397 | 重量% | 7.15 | 12.35 | 21.15 | 28.98 | 33.11 |
剪切粘度的测定
根据DIN标准53019第1和第3部分,测定剪切粘度。将润滑脂样品转移到各三个不锈钢制蒸发损失皿中。皿的几何参数描述在用于测定蒸发损失的标准(DIN 58397)中。随后将皿在具有循环的常规实验室干燥箱中在相应的试验温度(在此为200℃)下干燥。在每种情况下预定的持续时间(48 h、96 h、144 h和168 h)后,将皿从干燥箱中取出并使其冷却。在经受热应力之前测定各润滑脂的剪切粘度的起始值。
用测定润滑剂的流变参数的标准仪器(例如Anton Paar的MCR 302流变仪)进行剪切粘度的测量。
在此使用锥板系统(DIN EN ISO 3219和DIN 53019),其优选具有直径25 mm的测量锥。润滑脂样品的所需量取决于流变测量所需的典型量。测量持续时间是120秒,其中60秒是调温/保持时间。在300 1/s的恒定剪切速率和25℃的温度下进行测量。在90秒后可读出的值代表各润滑脂样品的剪切粘度。由测定的三个单独值形成平均值并最终示出。
表4
B1 | B2 | B3 | B4 | B5 | |||
剪切粘度起始值 | DIN 53019-1, -3 | mPas | 7557 | 7253 | 7210 | 6849 | 6106 |
剪切粘度48h/200℃ | DIN 53019-1, -3 | mPas | 6848 | 9857 | 9210 | 8651 | 5091 |
剪切粘度96h/200℃ | DIN 53019-1, -3 | mPas | 7671 | 10479 | 10292 | 9624 | 6587 |
剪切粘度144h/200℃ | DIN 53019-1, -3 | mPas | 6800 | 11764 | 11112 | 9986 | 8917 |
剪切粘度168h/200℃ | DIN 53019-1, -3 | mPas | 7494 | 10994 | 15452 | 9340 | 13623 |
实施例1至5的润滑脂现在与对比例 1和2的润滑脂和两种单独润滑脂(A)和(B)进行热耐受性的比较。结果显示在表5和6中。
表5
蒸发损失试验200℃ | VG1 | VG2 | 润滑脂A | 润滑脂B | ||
蒸发损失48h/200℃ | DIN 58397 | 重量% | 10.43 | 11.98 | 17.87 | 0.88 |
蒸发损失96h/200℃ | DIN 58397 | 重量% | 13.47 | 14.17 | 24.75 | 1.11 |
蒸发损失144h/200℃ | DIN 58397 | 重量% | 17.03 | 16.70 | 31.39 | 1.30 |
蒸发损失168h/200℃ | DIN 58397 | 重量% | 20.67 | 19.18 | 37.66 | 1.45 |
表6
VG1 | VG2 | 润滑脂A | 润滑脂B | |||
剪切粘度起始值 | DIN 53019-1, -3 | mPas | 5913 | 11880 | 6095 | 5966 |
剪切粘度48h/200℃ | DIN 53019-1, -3 | mPas | 9400 | 45976 | 7801 | 5800 |
剪切粘度96h/200℃ | DIN 53019-1, -3 | mPas | 12844 | 100000 | 8317 | 7104 |
剪切粘度144h/200℃ | DIN 53019-1, -3 | mPas | 18286 | 100000 | 7737 | 12093 |
剪切粘度168h/200℃ | DIN 53019-1, -3 | mPas | 35172 | 100000 | 8365 | 16025 |
上述结果表明,对于根据本发明的锂复合杂化润滑脂,剪切粘度的增加明显低于对比VG1和VG2。VG2在96小时后已表现出100000 mPas的剪切粘度并且不再能够润滑。在168小时的试验时间后,VG1表现出的剪切粘度是所有根据本发明的组合物B1至B5的两倍高,见表4。
PFPE/PTFE润滑脂(润滑脂B)如预期在该试验中表现出最低蒸发损失。令人惊讶地,根据本发明的实施例B1、B2和B4的剪切粘度在168小时的试验时间后低于润滑脂B并因此表现出更有利的硬化行为。
总体上表明,根据本发明的润滑剂在高温下的硬化行为比脲杂化润滑脂更有利。甚至已经令人惊讶地发现,一些根据本发明的组合物甚至表现出比PFPE/PTFE润滑脂更低的硬化。还已经令人惊讶地发现,根据本发明的润滑剂的油分离行为可通过润滑脂A(锂复合润滑脂)和B(PTFE/PFPE润滑脂)的特定混合比的选择进行设定,并因此适应不同的要求。
实施例2
用不同生产方法生产根据本发明的润滑剂
如上所述,根据本发明的润滑剂可以不同方式生产。在“在容器中混合”变体中,分开生产锂复合润滑脂(润滑脂C)和PFPE/PTFE润滑脂(润滑脂D),然后在40重量%比60重量%的比率下在容器中通过搅拌混合。所得锂复合杂化润滑脂B6随后使用三辊磨均质化。
在“原位生产”中,锂复合润滑脂的生产与润滑脂C相同,但在冷却时随后不同地也加入润滑脂D的成分,因此在一个操作中生产根据本发明的润滑剂组合物。根据本发明的润滑剂组合物B6随后也进行辊磨。
润滑脂C
作为基础油,生产由80重量%的来自烷基二苯醚(在40℃下100 mm2/sec)和偏苯三酸酯和完全氢化的聚异丁烯(完全氢化,Mn大约1300 g/mol)的混合物组成的锂复合润滑脂,以得到100 mm2/sec的在40℃下的粘度。提供15重量%的来自壬二酸和12-羟基硬脂酸的锂复合物和5重量%的由胺类抗氧化剂和磷酸酯组成的添加剂套装。工作后针入度为327 1/10 mm。
润滑脂D
生产含有65重量%的来自直链和支化PFPE的混合物(在40℃下的动态粘度145mm2/sec)、33重量%的PTFE微粉(平均粒度d50(激光衍射,DIN ISO 9277)大约5 µm、比表面积(DIN ISO 9277)大约5 m2/g)和2重量%的作为抗腐蚀添加剂的癸二酸二钠的PFPE/PTFE润滑脂。工作后针入度为286 1/10 mm。
表7
根据实施例2的根据本发明的实施例B6的数据.
参数/润滑脂 | 在容器中混合 | 原位煮制 |
工作后针入度60 dT [1/10 mm] (DIN ISO 2137) | 298 | 265 |
滴点[℃] (DIN ISO 2176) | > 300 | 277 |
100000 dT后的Δ工作后针入度[1/10 mm] (DIN ISO 2137) | 25 | 36 |
流动压力-40℃ [毫巴] (DIN 51805) | 550 | 725 |
流动压力-50℃ [毫巴] (DIN 51805) | 1025 | 1250 |
在25℃、剪切速率300 1/s下的剪切粘度[mPa*s] (DIN 53019-1, -3) | 4392 | 5378 |
蒸发损失,24h/150℃ [重量%] (DIN 58397) | 0.46 | 0.50 |
油分离,30h/150℃ [重量%] (ASTM D 6184) | 0.44 | 1.47 |
油分离,72h/150℃ [重量%] (ASTM D 6184) | 0.53 | 2.11 |
油分离,168h/40℃ [重量%] (DIN 51817) | 1.15 | 0.84 |
耐水性,静态,3h/90℃ (DIN 51807) | 0 | 0 |
铜腐蚀,24h/120℃ (DIN 51811) | 1 | 1 |
表8
蒸发损失试验220℃ | 在容器中混合 | 原位煮制 | ||
蒸发损失,48h/220℃ | DIN 58397 | 重量% | 11.37 | 10.67 |
蒸发损失,96h/220℃ | DIN 58397 | 重量% | 15.84 | 15.15 |
蒸发损失,144h/220℃ | DIN 58397 | 重量% | 20.65 | 19.48 |
蒸发损失,168h/220℃ | DIN 58397 | 重量% | 23.02 | 21.65 |
表9
在容器中混合 | 原位煮制 | |||
剪切粘度,起始值 | (DIN 53019-1, -3) | mPas | 4392 | 5378 |
剪切粘度,48h/220℃ | (DIN 53019-1, -3) | mPas | 6848 | 5823 |
剪切粘度,96h/220℃ | (DIN 53019-1, -3) | mPas | 6449 | 7732 |
剪切粘度,144h/220℃ | (DIN 53019-1, -3) | mPas | 10892 | 9342 |
剪切粘度,168h/220℃ | (DIN 53019-1, -3) | mPas | 10927 | 11753 |
这两种生产变体提供在测量精确度范畴内相等的值。
由于当前数据,根据生产实施例1和生产实施例2的B6可以通过这两种生产变体用作润滑剂。
因此表明,根据本发明的润滑剂组合物可通过不同方法生产。
Claims (14)
1.锂复合杂化润滑脂,其含有
(A) 70重量%至7重量%的酯或酯混合物,其选自偏苯三酸酯、均苯四酸酯、氢化或未氢化的二聚酸、交内酯,所述偏苯三酸酯包含作为烷氧基的含有6至18个碳原子,优选8至14个碳原子的直链或支化烷基,其中烷氧基可以相同或不同,
(B) 0.5重量%至20重量%的未氢化、氢化或完全氢化的聚异丁烯或其混合物,
(C) 1重量%至18重量%的锂复合皂和
(D) 5重量%至70重量%的全氟聚醚(PFPE)。
2.如权利要求1中所述的锂复合杂化润滑脂,其进一步含有
(E) 1重量%至30重量%的附加增稠剂。
3.如前述权利要求任一项中所述的锂复合杂化润滑脂,其进一步含有
(F) 0重量%至20重量%,优选2重量%至20重量%的附加油组分。
4.如前述权利要求任一项中所述的锂复合杂化润滑脂,其进一步含有
(G) 0重量%至10重量%,优选0.1重量%至10重量%的添加剂。
5.如前述权利要求任一项中所述的锂复合杂化润滑脂,其进一步含有
(H) 0重量%至10重量%,优选2重量%至5重量%的固体润滑剂。
6.如前述权利要求任一项中所述的锂复合杂化润滑脂,其特征在于组分(A)的均苯四酸酯是四(2-乙基己基)均苯四酸酯,且二聚酸是双(2-乙基己基)二聚酸酯。
7.如权利要求2中所述的锂复合杂化润滑脂,其特征在于组分(E)选自Al复合皂、不含锂的周期表第一和第二主族元素的金属单皂、不含锂的周期表第一和第二主族元素的金属复合皂、膨润土、磺酸盐、硅酸盐、气相二氧化硅、聚酰亚胺、PTFE或其混合物。
8.如权利要求3中所述的锂复合杂化润滑脂,其特征在于组分(F)选自矿物油、烷基化苯、烷基化萘、脂族羧酸酯和二羧酸酯、脂肪酸甘油三酯、烷基化二苯醚、间苯三酚酯和/或聚α-烯烃、α-烯烃共聚物、茂金属催化的聚α-烯烃。
9.如权利要求4中所述的锂复合杂化润滑脂,其特征在于组分(G)选自抗腐蚀添加剂、抗氧化剂、抗磨添加剂、紫外线稳定剂。
10.如权利要求5中所述的锂复合杂化润滑脂,其特征在于组分(H)选自BN、焦磷酸盐、氧化锌、氧化镁、焦磷酸盐、硫代硫酸盐、碳酸镁、碳酸钙、硬脂酸钙、硫化锌、硫化钼、硫化钨、硫化锡、石墨、石墨烯、纳米管、SiO2变型或其混合物。
11.如前述权利要求任一项中所述的锂复合杂化润滑脂用于润滑部件,特别是在车辆技术、轨道车辆、输送技术、膜拉伸装置、瓦楞纸板装置中的滚动轴承、滑动轴承、传递和正时链中的部件,滑轮轴承、风扇轴承、牵引发动机的轴承、用于润滑锥齿轮和正齿轮传动装置、弹簧、螺杆和压缩机、气动组件、阀和机器部件以及在偶尔无意与食品发生接触的装置中的用途。
12.将部件,特别是在车辆技术和轨道车辆中的滚动轴承、滑动轴承、传递和正时链中的部件润滑或上油的方法,所述方法包括:
将润滑剂组合物施加到所述部件的表面上,所述润滑剂包含:
(A) 70重量%至7重量%的酯或酯混合物,其选自偏苯三酸酯、均苯四酸酯、氢化或未氢化的二聚酸、交内酯,所述偏苯三酸酯包含作为烷氧基的含有6至18个碳原子,优选8至14个碳原子的直链或支化烷基,其中烷氧基可以相同或不同,
(B) 0.5重量%至20重量%的未氢化、氢化或完全氢化的聚异丁烯或其混合物,
(C) 1重量%至18重量%的锂复合皂和
(D) 5重量%至70重量%的全氟聚醚(PFPE)。
13.将连铸装置中的滑轮轴承、连续加热炉中的输送滚柱轴承、回转炉、管式磨、转鼓和混合器中的开放齿圈、瓦楞纸板装置或膜拉伸装置中的轴承或用于生产和运输食品的装置中的轴承润滑或上油的方法,所述方法包括:
将润滑剂组合物施加到所述部件的表面上,所述润滑剂包含:
(A) 70重量%至7重量%的酯或酯混合物,其选自偏苯三酸酯、均苯四酸酯、氢化或未氢化的二聚酸、交内酯,所述偏苯三酸酯包含作为烷氧基的含有6至18个碳原子,优选8至14个碳原子的直链或支化烷基,其中烷氧基可以相同或不同,
(B) 0.5重量%至20重量%的未氢化、氢化或完全氢化的聚异丁烯或其混合物,
(C) 1重量%至18重量%的锂复合皂和
(D) 5重量%至70重量%的全氟聚醚(PFPE)。
14.在连铸装置中的滑轮轴承、连续加热炉中的输送滚柱轴承、回转炉、管式磨、转鼓和混合器中的开放齿圈、瓦楞纸板装置或膜拉伸装置中的轴承、用于生产和运输食品的装置中的轴承上减少润滑脂在200℃下的硬化和/或减少润滑脂的油分离的方法,所述方法包括:
将润滑剂组合物施加到所述部件的表面上,所述润滑剂包含:
(A) 70重量%至7重量%的酯或酯混合物,其选自偏苯三酸酯、均苯四酸酯、氢化或未氢化的二聚酸、交内酯,所述偏苯三酸酯包含作为烷氧基的含有6至18个碳原子,优选8至14个碳原子的直链或支化烷基,其中烷氧基可以相同或不同,
(B) 0.5重量%至20重量%的未氢化、氢化或完全氢化的聚异丁烯或其混合物,
(C) 1重量%至18重量%的锂复合皂和
(D) 5重量%至70重量%的全氟聚醚(PFPE)。
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- 2021-02-03 EP EP21704440.3A patent/EP4090723B1/de active Active
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DE102020112993A1 (de) | 2021-11-18 |
US20230138681A1 (en) | 2023-05-04 |
WO2021228442A1 (de) | 2021-11-18 |
CN115461434B (zh) | 2024-03-22 |
EP4090723A1 (de) | 2022-11-23 |
EP4090723B1 (de) | 2023-11-29 |
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