EP0084910A2 - Lärmverhinderde Eigenschaften aufweisendes Lithium-Komplex-Fett mit hohem Tropfpunkt - Google Patents

Lärmverhinderde Eigenschaften aufweisendes Lithium-Komplex-Fett mit hohem Tropfpunkt Download PDF

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Publication number
EP0084910A2
EP0084910A2 EP83200077A EP83200077A EP0084910A2 EP 0084910 A2 EP0084910 A2 EP 0084910A2 EP 83200077 A EP83200077 A EP 83200077A EP 83200077 A EP83200077 A EP 83200077A EP 0084910 A2 EP0084910 A2 EP 0084910A2
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EP
European Patent Office
Prior art keywords
lithium
component
acid
group
composition
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
EP83200077A
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English (en)
French (fr)
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EP0084910A3 (en
EP0084910B1 (de
Inventor
Norimitsu Tanaka
Hiroshi Tajiri
Toshiko Okamoto
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.)
Shell Internationale Research Maatschappij BV
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Shell Internationale Research Maatschappij BV
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Priority claimed from JP675782A external-priority patent/JPS58125794A/ja
Priority claimed from JP675882A external-priority patent/JPS58125795A/ja
Application filed by Shell Internationale Research Maatschappij BV filed Critical Shell Internationale Research Maatschappij BV
Publication of EP0084910A2 publication Critical patent/EP0084910A2/de
Publication of EP0084910A3 publication Critical patent/EP0084910A3/en
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Publication of EP0084910B1 publication Critical patent/EP0084910B1/de
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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
    • C10N2060/00—Chemical after-treatment of the constituents of the lubricating composition
    • C10N2060/04—Oxidation, e.g. ozonisation

Definitions

  • the present invention relates to a high-quality lithium-complex grease composition having improved anti-noise properties, a high dropping point, a long lubrication life and an excellent oxidation stability also at high temperatures.
  • lithium-complex greases High dropping-point lithium-soap greases are generally referred to as lithium-complex greases, and several of them are proposed so far (see e.g. US patent specifications 2,940,930, 3,223,624, 3,758,407 and 3,929,651).
  • these lithium-complex greases were inferior in their anti-noise properties because of the low dispersancy in the base oils of the metal salts used for the formation of complexes with lithium soaps.
  • the purpose of the present invention is to provide a lithium-complex grease composition having a long lubrication life, markedly improved anti-noise properties, a high dropping point, and an excellent oxidation stability also at high temperatures, by uniformly admixing and dispersing in a base lubricating oil a gelling agent (a), a complexing metal salt (b) and a dispersing component (c).
  • This invention therefore relates to a high dropping-point lithium-complex grease composition having improved anti-noise properties, comprising a lubricating oil and the following components:
  • component (c) results into unexpectedly superior grease properties compared with the known greases which do not contain this component (c).
  • Any conventional lubricating oil can be used. While a typical one is a mineral oil, use can also be made, singly or in combination with the mineral oil, of a synthetic oil including ester oils, such as a diester oil, e.g. dioctyl azelate, and a tetra-ester oil, e.g.
  • V.I. viscosity index
  • the lubricating oil may have a viscosity ranging from about 2 to 500 cSt, preferably from 20 to 200 cSt, at 40°C.
  • the C 10 to C 34 fatty acids include the saturated or unsaturated higher aliphatic monocarboxylic acids, especially those acids containing 16 to 22 carbon atoms, such as stearic acid and oleic acid.
  • the C 12 to C 24 hydroxy fatty acids include saturated or unsaturated monocarboxylic fatty acids containing a hydroxyl radical, especially those acids containing I8 carbon atoms and a hydroxyl radical in the 9-, 10- or 12-position, such as 12-hydroxy stearic acid and ricinolic acid.
  • the lithium salts of the above fatty acids and hydroxy fatty acids can be singly used or combinedly with one or more of others.
  • said carboxylic acids can be reacted with lithium hydroxide not only in the form of free acids but also as glycerides.
  • Suitable C 4 to C 12 dicarboxylic acids used in the formation of the dilithium salt are e.g. succinic acid, glutaric acid, adipic acid, suberic acid, pimelic acid, azelaic acid, dodecane dionic acid and sebacic acid. Acids containing 6 to 10 carbon atoms, especially adipic acid, sebacic acid and azelaic acid, are preferred.
  • the lithium salts of boric acids can be used in place ot or in combination with said dilithium salt or the other lithium salt.
  • Suitable boric acid salts are lithium metaborate, lithium tetraborate lithium pentaborate, lithium perborate and the monolithium salt of ortho boric acid (H 3 B 0 3 ).
  • the lithium salt of an aromatic hydroxy carboxylic acid can be used in place of or in combination with the above components (b).
  • Suitable acids have the formula: wherein R is a hydrogen atom or a hydroxyl, lower alkyl or lower alkoxy radical.
  • Such acids include p-hydroxy benzoic acid, salicyclic acid (o-hydroxy benzoic acid), 2-hydroxy-4-hexyl benzoic acid, m-hydroxy benzoic acid,'2,5-dihydroxyl benzoic acid (gentisic acid), 2,6-dihydroxyl benzoic acid (y-resorcylic acid) and 4-hydroxy-3-methoxy benzoic acid.
  • Salicylic acid is preferred.
  • the hydroxyl radical (OH) in said lithium salt can he present in its free state as well as in the form of -OLi.
  • This component is used for the acceleration of the fine dispersion of the components (a) and (b) in the base oil, and the high-molecular VI-improver, succinic-imide type dispersant and metal salt detergent can be employed singly or combinedly with one or more of other ones.
  • Suitable high-molecular VI-improvers are oil-soluble high-molecular compounds having a mean molecular weight of about 1,000 to 1,500,000 in general, preferably about 2,000 to 300,000, and they reduce the temperature-dependency of the oil viscosity. Any of the conventional VI-improvers can be used, such as:
  • oil-soluble high-molecular compounds particularly preferred are those methyl-methacrylate polymers of the mean molecular weights fanging from 100,000 to 200,000, hydrogenated styrene-butadiene copolymers of the mean molecular weights ranging from 80,000 to 160,000 hydrogenated styrene-isoprene copolymers of the mean molecular weights ranging from 80,000 to 160,000, ethylene-propylene copolymers of the mean molecular weights ranging from 80,000 to 160,000 and mixtures of theem.
  • Suitable succinimide type dispersants are synthezised by reaction of polyamines with the polybutenyl succinic anhydrides obtained by the reaction of polybutenes and maleic anhydride. They include those dispersants represented respectively by the following formulae: and wherein A 1 denotes a C 30 to C 200 polyisobutenyl radical, p means an integer from 2 to 8 and q represents an integer from 1 to 8.
  • Suitable metal salt detergents include sulphonates, phenates, phosphonates and salicylates represented respectively by the following formulae:
  • calcium sulphonate calcium phenate
  • calcium salicylate calcium salicylate
  • magnesium salicylate are preferred.
  • Metal naphtenates can also be used.
  • the above metal salts may be neutral, basic or super-basic. Combinations of the metal salts may also be suitable.
  • the grease composition according to the present invention can be prepared by uniformly admixing and finely dispersing the three components (a), (b) and (c) in the base oil mentioned above. While the amounts of these three components compounded in the base oil above are not necessarily critical but can be variable for individual components, it is generally advantageous to use them in the following proportions per 100 weight parts (pbw) of the base oil;
  • Component(a)/Component(b) mol ratio 0.5 to 10, especially 1 to 5.
  • lubricant-additives such as neutral or basic metallic detergents, such as basic Ca salicylate, or ashless dispersants, rust inhibitors (e.g., paraffin oxide, amino imidazoline or barium dinonylnaphthalene-sulphonate), oxidation inhibitors (e.g. 2,6-ditertiary butyl-4-methylphenol, N-phenyl-a-naphthylamine or diphenylamine octylate) and extreme-pressure additives (e.g. zinc naphthenate, or other zinc compounds such as zinc dithiophosphates or zinc-oxide, lead naphthenate, sulphurized oils and fats, or tricresyl phosphate), in the proportions ordinarily employed.
  • neutral or basic metallic detergents such as basic Ca salicylate, or ashless dispersants
  • rust inhibitors e.g., paraffin oxide, amino imidazoline or barium dinonylnaphthalen
  • the grease composition of the present invention can e.g. be prepared in the following manner.
  • a component (c) is first admixed and dissolved in a base oil, and the fatty acid or hydroxy fatty acid for the preparation of the lithium soap, as a component (a), is admixed and dissolved in the mixture thus obtained, at 70 to 80°C. Then, the lithium hydroxide roughly in an equivalent amount to the fatty acid or hydroxy fatty acid above is admixed in the resulting mixture at 80 to 90°C to form a soap, and the mixture is further heated to 140 to 150°C under pressure for dehydration.
  • the resulting mixture is cooled to 80 to 100°C and further admixed with the lithium hydroxide roughly in an equivalent amount to said dicarboxylic acid or boric acid, and the final mixture is again dehydrated by heating to 140 to 150°C under pressure.
  • the last dehydrated mixture is further heated to 195 to 215°C, then cooled to 175 to 193°C, maintained at this temperature for about 10 to 40 min. and finally cooled to the room temperature.
  • the lithium-complex grease composition according to the present invention and thus prepared has a very high dropping point, satisfactory anti-noise properties and very long lubricating life and exhibits exceedingly high performance as a lubricating grease.
  • the present composition possesses a very high extreme-pressure property, in addition to the excellent properties above, due to the lithium borate contained as the component (b). Therefore, the present grease composition can be suitably used, for example, for the lubrication of the bearings fitted in electric motors as well as of the wheel bearings in automotive bearing/axle integrated structures. Furhtermore, these greases make little noise even if used in the bearings of air-conditioners and others, giving no environmental injury.
  • the contents were admixed with 67.8 g of azelaic acid, the mixture was slowly cooled to about 90°C under stirring, and 250 g of a hot aqueous solution (95°C) containing 30.2 g of lithium hydroxide were admixed in the mixture.
  • the resulting mixture was slowly heated to 145 to 155°C under stirring and pressure in 1 to 1.5 hrs, and, at this temperature, the autoclave was released of the pressure and removed of the moisture.
  • the contents of the autoclave were again heated to I95 to 215°C and, then, left cooling under stirring to 188 to 192°C.
  • the contents were kept at this temperature for 20 to 30 min, then left cooling to about 160°C.
  • 60 g of the oxidation inhibitor, diphenylamine octylate were admixed in the contents, the mixture was cooled to about 80 to 85°C under stirring in 30 to 60 min and treated in a homogenizer at this temperature.
  • a grease composition was prepared in a similar manner to that in Example 1 except that 2,533.5 g of the refined mineral oil were used without employing the hydrogenated styrene-butadiene copolymer mentioned in Example 1.
  • the properties of the product were as follows;
  • Grease compositions were prepared by employing the various components shown in Table 1 below in a similar manner to that in Example 1, and the properties of these compositions are collectively tabularized in Table 1.
  • Grease compositions were prepared by treating the various components shown in following Tables 2A and 2B in similar manners to that in Example 1. The properties of these compositions are shown collectively in Tables 2A and 2B.
  • Grease compositions were prepared by treating the various components shown in following Table 3 in similar manners to that in Example 1. The properties of these compositions are collectively tabularized in Table 3.
  • the autoclave was released of the pressure and the contents were dehydrated at this temperature in 15 to 25 min. After the dehydration, the contents of the autoclave were further heated to 195 to 205°C, then cooled to 188 to 192°C under stirring and, after being kept at this temperature for 20 to 30 min, further cooled to about 160°C. At this temperature, 60 g of an oxidation inhibitor were admixed in the contents, the mixture thus obtained was cooled by stirring to about 80 to 85°C in 30 to 60 min and then treated in a homogenizer at this temperature.
  • the properties of the grease composition thus prepared were as follows:
  • a grease composition was prepared in a similar manner to that in Example 1 except that 2,531.2 g of the refined mineral oil were employed without the succinimide(A) being admixed.
  • the properties of the resulting composition were as follows;
  • Table 4 Seven grease compositions were prepared by treating the various components shown in Table 4 below in similar ways to that in Example 26 and the properties thereof are collectively tabularized in Table 4. Also, the properties of a market grease comprising the lithium soap of 12-hydroxystearic acid are shown as * Comparison Example 5 in the table as well.
  • Comparison Example 6 in the Table is a grease prepared in a similar manner to that in Example 26 but by employing in a similar manner to that in Example 26 but by employing an increase amount of the refined mineral oil without the components (b) and (c) being admixed.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Lubricants (AREA)
EP83200077A 1982-01-21 1983-01-18 Lärmverhinderde Eigenschaften aufweisendes Lithium-Komplex-Fett mit hohem Tropfpunkt Expired EP0084910B1 (de)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP6758/82 1982-01-21
JP675782A JPS58125794A (ja) 1982-01-21 1982-01-21 音響特性が改善された高滴点リチウムコンプレツクスグリ−ス組成物
JP6757/82 1982-01-21
JP675882A JPS58125795A (ja) 1982-01-21 1982-01-21 高滴点リチウムコンプレツクスグリ−ス組成物

Publications (3)

Publication Number Publication Date
EP0084910A2 true EP0084910A2 (de) 1983-08-03
EP0084910A3 EP0084910A3 (en) 1985-01-16
EP0084910B1 EP0084910B1 (de) 1989-02-22

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AU (1) AU554600B2 (de)
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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0191608A2 (de) * 1985-02-09 1986-08-20 The British Petroleum Company p.l.c. Schmierfett für Steinbohrerspitzen und so geschmierte Bohrerspitzen
EP0227182A2 (de) * 1985-12-23 1987-07-01 Shell Internationale Researchmaatschappij B.V. Fettzusammensetzung
GB2215346A (en) * 1988-03-09 1989-09-20 Exxon Research Engineering Co Lithium complex lubricating grease
EP0405892A2 (de) * 1989-06-27 1991-01-02 Exxon Research And Engineering Company Wasserbeständige Schmierfettzusammensetzung
EP0580335A1 (de) * 1992-07-10 1994-01-26 The Lubrizol Corporation Schmierfettzusammensetzungen
US5362409A (en) * 1992-07-10 1994-11-08 The Lubrizol Corporation Grease compositions
WO1995035355A1 (en) * 1994-06-17 1995-12-28 Exxon Research And Engineering Company Grease composition
KR960022967A (ko) * 1994-12-22 1996-07-18 야마자키 야스시 윤활 첨가제 및 이를 함유하는 윤활 그리이스 조성물
US5558807A (en) * 1995-05-19 1996-09-24 Exxon Research And Engineering Company Wax isomerate-based high temperature long bearing life grease
WO1999042541A1 (en) * 1998-02-17 1999-08-26 Exxon Research And Engineering Company Lubricating grease composition and preparation
US6063742A (en) * 1999-03-01 2000-05-16 The Lubrizol Corporation Grease compositions
US6100226A (en) * 1998-05-20 2000-08-08 The Lubrizol Corporation Simple metal grease compositions
US6214778B1 (en) 1995-08-24 2001-04-10 The Lubrizol Corporation Polyurea-thickened grease composition
US6300288B1 (en) 1994-03-31 2001-10-09 The Lubrizol Corporation Functionalized polymer as grease additive
US20120004153A1 (en) * 2010-06-30 2012-01-05 Chevron U.S.A. Inc. Lithium Complex Grease with Improved Thickener Yield
US9029307B2 (en) 2010-12-16 2015-05-12 Invista North America S.A R.L. Thickened grease composition
CN108130168A (zh) * 2017-12-28 2018-06-08 东莞太平洋博高润滑油有限公司 一种高温锂基脂及其制备方法
WO2018164979A1 (en) * 2017-03-06 2018-09-13 The Lubrizol Corporation Fuel additives

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102051257B (zh) * 2010-12-31 2013-04-17 鞍山海华油脂化学有限公司 复合锂基润滑脂及其生产工艺

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US3929651A (en) * 1970-11-18 1975-12-30 Exxon Research Engineering Co Modified lithium soap grease
US3929650A (en) * 1974-03-22 1975-12-30 Chevron Res Extreme pressure agent and its preparation
US4100080A (en) * 1977-03-14 1978-07-11 Chevron Research Company Greases containing borate dispersions as extreme-pressure additives
US4156655A (en) * 1978-01-30 1979-05-29 Exxon Research & Engineering Co. Grease composition resistant to salt water corrosion

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US3929651A (en) * 1970-11-18 1975-12-30 Exxon Research Engineering Co Modified lithium soap grease
US3929650A (en) * 1974-03-22 1975-12-30 Chevron Res Extreme pressure agent and its preparation
US4100080A (en) * 1977-03-14 1978-07-11 Chevron Research Company Greases containing borate dispersions as extreme-pressure additives
US4156655A (en) * 1978-01-30 1979-05-29 Exxon Research & Engineering Co. Grease composition resistant to salt water corrosion

Cited By (35)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0191608A3 (de) * 1985-02-09 1988-07-27 The British Petroleum Company p.l.c. Schmierfett für Steinbohrerspitzen und so geschmierte Bohrerspitzen
EP0191608A2 (de) * 1985-02-09 1986-08-20 The British Petroleum Company p.l.c. Schmierfett für Steinbohrerspitzen und so geschmierte Bohrerspitzen
EP0227182A2 (de) * 1985-12-23 1987-07-01 Shell Internationale Researchmaatschappij B.V. Fettzusammensetzung
US4719023A (en) * 1985-12-23 1988-01-12 Shell Oil Company Grease composition
EP0227182A3 (en) * 1985-12-23 1988-08-10 Shell Internationale Research Maatschappij B.V. Crease composition
GB2215346B (en) * 1988-03-09 1991-09-04 Exxon Research Engineering Co Lubricating grease
GB2215346A (en) * 1988-03-09 1989-09-20 Exxon Research Engineering Co Lithium complex lubricating grease
EP0405892A2 (de) * 1989-06-27 1991-01-02 Exxon Research And Engineering Company Wasserbeständige Schmierfettzusammensetzung
EP0405892A3 (de) * 1989-06-27 1991-01-16 Exxon Research And Engineering Company Wasserbeständige Schmierfettzusammensetzung
US5110489A (en) * 1989-06-27 1992-05-05 Exxon Research And Engineering Company Water resistant grease composition
EP0580335A1 (de) * 1992-07-10 1994-01-26 The Lubrizol Corporation Schmierfettzusammensetzungen
US5362409A (en) * 1992-07-10 1994-11-08 The Lubrizol Corporation Grease compositions
EP0651043A2 (de) * 1993-10-25 1995-05-03 The Lubrizol Corporation Schmierfettzusammensetzungen
EP0651043A3 (de) * 1993-10-25 1995-08-30 Lubrizol Corp Schmierfettzusammensetzungen.
US6300288B1 (en) 1994-03-31 2001-10-09 The Lubrizol Corporation Functionalized polymer as grease additive
WO1995035355A1 (en) * 1994-06-17 1995-12-28 Exxon Research And Engineering Company Grease composition
EP0718394A3 (de) * 1994-12-22 1996-10-09 Showa Shell Sekiyu Schmiermitteladditiv und diese enthaltende Schmierfettzusammensetzung
US5877129A (en) * 1994-12-22 1999-03-02 Showa Shell Sekiyu K.K. Lubricant additive and lubricating grease composition containing the same
AU705469B2 (en) * 1994-12-22 1999-05-20 Showa Shell Sekiyu K.K. Lubricant additive and lubricating grease composition containing the same
KR960022967A (ko) * 1994-12-22 1996-07-18 야마자키 야스시 윤활 첨가제 및 이를 함유하는 윤활 그리이스 조성물
US5558807A (en) * 1995-05-19 1996-09-24 Exxon Research And Engineering Company Wax isomerate-based high temperature long bearing life grease
US6214778B1 (en) 1995-08-24 2001-04-10 The Lubrizol Corporation Polyurea-thickened grease composition
AU743979B2 (en) * 1998-02-17 2002-02-14 Exxon Research And Engineering Company Lubricating grease composition and preparation
WO1999042541A1 (en) * 1998-02-17 1999-08-26 Exxon Research And Engineering Company Lubricating grease composition and preparation
US6407043B1 (en) 1998-02-17 2002-06-18 Exxonmobil Research And Engineering Company Lubricating grease composition and preparation
US6100226A (en) * 1998-05-20 2000-08-08 The Lubrizol Corporation Simple metal grease compositions
US6063742A (en) * 1999-03-01 2000-05-16 The Lubrizol Corporation Grease compositions
US20120004153A1 (en) * 2010-06-30 2012-01-05 Chevron U.S.A. Inc. Lithium Complex Grease with Improved Thickener Yield
WO2012005799A2 (en) 2010-06-30 2012-01-12 Chevron U.S.A. Inc. Lithium complex grease with improved thickener yield
WO2012005799A3 (en) * 2010-06-30 2012-03-15 Chevron U.S.A. Inc. Lithium complex grease with improved thickener yield
US9029307B2 (en) 2010-12-16 2015-05-12 Invista North America S.A R.L. Thickened grease composition
WO2018164979A1 (en) * 2017-03-06 2018-09-13 The Lubrizol Corporation Fuel additives
CN110382670A (zh) * 2017-03-06 2019-10-25 路博润公司 燃料添加剂
CN110382670B (zh) * 2017-03-06 2022-06-10 路博润公司 燃料添加剂
CN108130168A (zh) * 2017-12-28 2018-06-08 东莞太平洋博高润滑油有限公司 一种高温锂基脂及其制备方法

Also Published As

Publication number Publication date
AU1067583A (en) 1983-07-28
AU554600B2 (en) 1986-08-28
EP0084910A3 (en) 1985-01-16
EP0084910B1 (de) 1989-02-22
DE3379227D1 (en) 1989-03-30

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