CN109370723B - High-antifriction-performance composite calcium sulfonate-based lubricating grease and preparation method thereof - Google Patents
High-antifriction-performance composite calcium sulfonate-based lubricating grease and preparation method thereof Download PDFInfo
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- CN109370723B CN109370723B CN201811330698.8A CN201811330698A CN109370723B CN 109370723 B CN109370723 B CN 109370723B CN 201811330698 A CN201811330698 A CN 201811330698A CN 109370723 B CN109370723 B CN 109370723B
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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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/045—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution and non-macromolecular compounds
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/05—Metals; Alloys
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
-
- 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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
-
- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
-
- 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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
- C10M2215/064—Di- and triaryl amines
-
- 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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
-
- 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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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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)
- Lubricants (AREA)
Abstract
The invention discloses a high antifriction performance composite calcium sulfonate-based lubricating grease which is mainly prepared from the following raw materials in parts by weight: 50 parts of high-base-number calcium sulfonate, 20-40 parts of base oil, 5-15 parts of alkyl benzene sulfonic acid, 0.5-1.5 parts of calcium carbonate, 0.5-1.5 parts of antioxidant and nano WS20.2 to 1 portion of superfine nickel powder and 0.4 to 2 portions of superfine nickel powder. Compared with the prior art, the composite calcium sulfonate-based lubricant has the advantages that the raw material cost is low, the formula is reasonable, the obtained composite calcium sulfonate-based lubricant has balanced various properties and can meet most of requirements, and more importantly, the friction reducing performance of the composite calcium sulfonate-based lubricant is outstanding and can meet some special requirements.
Description
Technical Field
The invention relates to a high antifriction performance composite calcium sulfonate base lubricating grease and a preparation method thereof, belonging to the technical field of composite calcium sulfonate base lubricating grease.
Background
The composite calcium sulfonate lubricating grease is a novel lubricating grease, has very comprehensive performance compared with other high-temperature lubricating greases, has excellent high-temperature performance, water resistance, extreme pressure wear resistance and antirust performance, and can meet the requirement of centralized lubrication in pumping performance. The lubricating effect under the harsh conditions of high temperature, much water, heavy load and the like is obviously superior to that of other lubricating grease, and the lubricating grease is particularly suitable for lubricating equipment in continuous casting machines, continuous rolling units and similar conditions of a steel mill, is favorable for simplifying the variety of the lubricating grease and is convenient for oil management. The specific applicable parts are as follows: a mining truck bearing; a main transmission bearing of a ball mill of a concentrating mill; a vibrating screen bearing of a sintering plant; coke car bearings in iron works; gear rings of ladle turntables of various continuous casting machines; a second cooling zone of the continuous casting machine, a fan-shaped section, a withdrawal and straightening machine and a conveying roller bearing; various strip mill knockout roll tables, roughing mill working rolls, finishing mill working rolls, recoiling machine bearings, tooth-shaped adapters and water pump bearings; forming rollers of a pipe mill in a seamless steel pipe factory; a furnace bottom roller way bearing of a working roll of a rolling mill of a medium plate factory and a heat treatment furnace; section bar, wire mill working roll, cooling bed bearing, etc. It is also suitable for lubricating other high-temperature, heavy-load and watery occasions, such as equipment in the industries of ships, fire resistance, chemical engineering, automobiles and the like.
The grease forming mechanism of the composite calcium sulfonate lubricating grease comprises the following steps: the high base number calcium petroleum sulfonate is converted into semisolid grease from liquid under the action of a conversion agent, and the semisolid grease is the calcium sulfonate lubricating grease. The high base number calcium petroleum sulfonate consists of diluent oil, calcium sulfonate and calcium carbonate (amorphous), wherein the calcium carbonate is wrapped by the calcium sulfonate to form a stable micelle, the diluent oil is distributed outside the calcium carbonate, and the whole system is in a stable and transparent liquid state. The conversion agent is generally a substance containing active hydrogen. Because the polarity of the conversion agent is stronger than that of calcium carbonate, calcium sulfonate can be dissociated from micelles to wrap the conversion agent, the original stable micelle system loses balance, and amorphous calcium carbonate is dissociated from micelles and is aggregated into calcite-shaped crystals under the comprehensive action of the conversion agent (including water). The reaction process is as follows: the conversion agent reacts with calcium carbonate to generate calcium salt (soap), carbon dioxide and water; generating calcium bicarbonate by using carbon dioxide, water and calcium carbonate; calcium bicarbonate is heated and then decomposed into calcium carbonate, carbon dioxide and water; in the process, carbon dioxide and water are recycled, and almost all calcium carbonate is finally dissociated from the stable micelles to form calcite-shaped crystals. The calcium carbonate crystals and the calcium sulfonate are mutually adsorbed to form colloidal particles or micelles with larger particle sizes, and the colloidal particles or micelles form an interlaced network skeleton (namely a gel structure) by virtue of molecular force and ionic force, so that the oil is fixed in gaps of the structure skeleton. A two-phase dispersion system comprising a base oil as a dispersion medium and oil-containing gel particles as a dispersion phase is formed, thereby forming a grease.
The compound calcium sulfonate lubricating grease is researched and applied in a large amount in the last 80 th century abroad, but the research in China is relatively late, so that the compound calcium sulfonate lubricating grease is mostly limited in documents at present and is rarely really industrialized. At present, the complex calcium sulfonate lubricating grease on the market is various, but the performance is mediocre and certain special requirements cannot be met.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides the composite calcium sulfonate-based lubricating grease with high antifriction performance and the preparation method thereof.
The technical scheme is as follows: in order to achieve the purpose, the invention adopts the following technical scheme:
a high antifriction performance composite calcium sulfonate base lubricating grease is mainly prepared from the following raw materials in parts by weight:
50 parts of high-base-number calcium sulfonate, 20-40 parts of base oil, 5-15 parts of alkyl benzene sulfonic acid, 0.5-1.5 parts of calcium carbonate, 0.5-1.5 parts of antioxidant and nano WS20.2 to 1 portion of superfine nickel powder and 0.4 to 2 portions of superfine nickel powder.
Preferably:
the total base number of the high-base-number calcium sulfonate is 350-450 mgKOH/g.
The base oil is mineral oil or synthetic oil, such as 150BS, 500SN, PAO.
The antioxidant is diphenylamine, dioctyl diphenylamine or di-tert-butyl-p-cresol.
The nano WS2The mass ratio of the superfine nickel powder to the superfine nickel powder is 1: 2.
The preparation method of the composite calcium sulfonate-based lubricating grease with high antifriction performance comprises the following steps:
(1) adding high-base-number calcium sulfonate, half of base oil, half of alkylbenzene sulfonic acid, calcium carbonate and water serving as solvents into a reaction kettle, heating and stirring;
(2) adding the balance of the base oil and the alkylbenzene sulfonic acid into a reaction kettle, heating and stirring;
(3) finally adding nano WS2And superfine nickel powder, and continuously stirring;
(4) removing the solvent under reduced pressure, and raising the temperature to 160-180 ℃ for refining;
(5) and cooling, adding an antioxidant, and further cooling to obtain the composite calcium sulfonate-based lubricating grease.
Preferably:
in the step (1), the heating temperature is 75-85 ℃, and the stirring time is 30-60 min.
In the step (2), the temperature for heating and stirring is 85-95 ℃, and the stirring time is 30-60 min.
The stirring time in the step (3) is 30-60min, and the refining time in the step (4) is 5-10 min.
Has the advantages that: compared with the prior art, the composite calcium sulfonate-based lubricant has the advantages that the raw material cost is low, the formula is reasonable, the obtained composite calcium sulfonate-based lubricant has balanced various properties and can meet most of requirements, and more importantly, the friction reducing performance of the composite calcium sulfonate-based lubricant is outstanding and can meet some special requirements.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
the formula is as follows:
50 parts of high-base-number calcium sulfonate, 20 parts of base oil, 5 parts of alkyl benzene sulfonic acid, 0.5 part of calcium carbonate, 0.5 part of antioxidant and nano WS20.2 part of superfine powder0.4 part of nickel powder.
The total base number of the high-base-number calcium sulfonate is 350mgKOH/g, the base oil is 150BS, and the antioxidant is diphenylamine.
The preparation method comprises the following steps:
(1) taking high-base-number calcium sulfonate, half of base oil, half of alkylbenzene sulfonic acid, calcium carbonate and water as solvents, adding the solvents into a reaction kettle, heating to 75 ℃, and stirring for 30 min;
(2) adding the balance of the base oil and the alkylbenzene sulfonic acid into a reaction kettle, heating to 85 ℃, and stirring for 30 min;
(3) finally adding nano WS2And the superfine nickel powder, and continuously stirring for 30 min;
(4) removing the solvent under reduced pressure, heating to 160 deg.C, and refining for 10 min;
(5) and cooling, adding an antioxidant, and further cooling to obtain the composite calcium sulfonate-based lubricating grease.
Example 2:
the formula is as follows:
50 parts of high-base-number calcium sulfonate, 40 parts of base oil, 15 parts of alkyl benzene sulfonic acid, 1.5 parts of calcium carbonate, 1.5 parts of antioxidant and nano WS21 part and 2 parts of superfine nickel powder.
The total base number of the high-base-number calcium sulfonate is 450mgKOH/g, the base oil is 500SN, and the antioxidant is dioctyl diphenylamine.
The preparation method comprises the following steps:
(1) taking high-base-number calcium sulfonate, half of base oil, half of alkylbenzene sulfonic acid, calcium carbonate and water as solvents, adding the solvents into a reaction kettle, heating to 85 ℃, and stirring for 60 min;
(2) adding the balance of the base oil and the alkylbenzene sulfonic acid into a reaction kettle, heating to 95 ℃, and stirring for 60 min;
(3) finally adding nano WS2Mixing with superfine nickel powder, and stirring for 60 min;
(4) removing the solvent under reduced pressure, heating to 180 deg.C, and refining for 5 min;
(5) and cooling, adding an antioxidant, and further cooling to obtain the composite calcium sulfonate-based lubricating grease.
Example 3:
the formula is as follows:
50 parts of high-base-number calcium sulfonate, 30 parts of base oil, 10 parts of alkyl benzene sulfonic acid, 1 part of calcium carbonate, 1 part of antioxidant and nano WS20.6 part and 1.2 parts of superfine nickel powder.
The total base number of the high-base-number calcium sulfonate is 400mgKOH/g, the base oil is PAO, and the antioxidant is di-tert-butyl-p-cresol.
The preparation method comprises the following steps:
(1) taking high-base-number calcium sulfonate, half of base oil, half of alkylbenzene sulfonic acid, calcium carbonate and water as solvents, adding the solvents into a reaction kettle, heating to 80 ℃, and stirring for 45 min;
(2) adding the balance of the base oil and the alkylbenzene sulfonic acid into a reaction kettle, heating to 90 ℃, and stirring for 45 min;
(3) finally adding nano WS2And the superfine nickel powder, and continuously stirring for 45 min;
(4) removing the solvent under reduced pressure, heating to 170 deg.C, and refining for 8 min;
(5) and cooling, adding an antioxidant, and further cooling to obtain the composite calcium sulfonate-based lubricating grease.
Example 4:
the formula is as follows:
50 parts of high-base-number calcium sulfonate, 25 parts of base oil, 8 parts of alkylbenzene sulfonic acid, 0.8 part of calcium carbonate, 0.7 part of antioxidant and nano WS20.4 part of superfine nickel powder and 0.8 part of superfine nickel powder.
The total base number of the high-base-number calcium sulfonate is 400mgKOH/g, the base oil is 150BS, and the antioxidant is diphenylamine.
The preparation method comprises the following steps:
(1) taking high-base-number calcium sulfonate, half of base oil, half of alkylbenzene sulfonic acid, calcium carbonate and water as solvents, adding the solvents into a reaction kettle, heating to 80 ℃, and stirring for 40 min;
(2) adding the balance of the base oil and the alkylbenzene sulfonic acid into a reaction kettle, heating to 90 ℃, and stirring for 40 min;
(3) finally adding nano WS2And the superfine nickel powder, and continuously stirring for 40 min;
(4) removing the solvent under reduced pressure, heating to 165 deg.C, and refining for 8 min;
(5) and cooling, adding an antioxidant, and further cooling to obtain the composite calcium sulfonate-based lubricating grease.
Example 5:
the formula is as follows:
50 parts of high-base-number calcium sulfonate, 35 parts of base oil, 12 parts of alkyl benzene sulfonic acid, 1.2 parts of calcium carbonate, 1.3 parts of antioxidant and nano WS20.8 part and 1.6 parts of superfine nickel powder.
The total base number of the high-base-number calcium sulfonate is 400mgKOH/g, the base oil is 500SN, and the antioxidant is dioctyl diphenylamine.
The preparation method comprises the following steps:
(1) taking high-base-number calcium sulfonate, half of base oil, half of alkylbenzene sulfonic acid, calcium carbonate and water as solvents, adding the solvents into a reaction kettle, heating to 80 ℃, and stirring for 50 min;
(2) adding the balance of the base oil and the alkylbenzene sulfonic acid into a reaction kettle, heating to 90 ℃, and stirring for 50 min;
(3) finally adding nano WS2And the superfine nickel powder, and continuously stirring for 50 min;
(4) removing the solvent under reduced pressure, heating to 175 deg.C, and refining for 6 min;
(5) and cooling, adding an antioxidant, and further cooling to obtain the composite calcium sulfonate-based lubricating grease.
And (3) performance detection:
1. the product obtained in the above example is subjected to performance detection, and the results are shown in the following table 1:
TABLE 1 results of product Performance test obtained in examples
2. And (3) friction reduction performance investigation:
the friction and wear performance of various products is researched by adopting a four-ball testing machine, and the appearance and the surface composition of the wear marks are analyzed by means of a Scanning Electron Microscope (SEM), an energy spectrum analysis (EDS), a Transmission Electron Microscope (TEM) and the like.
Comparative example 1 is substantially the same as inventive example 3 except that the raw material nano WS was not included2And ultrafine nickel powder.
Comparative example 2 is substantially the same as inventive example 3 except that the nano-WS was used2And the using amount of the superfine nickel powder is 1 part.
The experimental results show that: the greases of inventive examples 1-5 had friction coefficients that were reduced by 21.2%, 22.3%, 23.5%, 22.8%, and 22.1%, respectively, as compared to control example 1, and the greases of inventive examples 1-5 had friction coefficients that were reduced by 15.3%, 16.1%, 20.3%, 19.7%, and 19.5%, respectively, as compared to control example 2, indicating that although nano-WS was present2The addition of the superfine nickel powder can improve the antifriction performance, but the effect is not obvious, and the antifriction performance of the lubricating grease can be greatly improved by adopting the specific proportion in the invention.
Claims (2)
1. The composite calcium sulfonate-based lubricating grease with high friction reducing performance is characterized by being mainly prepared from the following raw materials in parts by weight:
50 parts of high-base-number calcium sulfonate, 20-40 parts of base oil, 5-15 parts of alkyl benzene sulfonic acid, 0.5-1.5 parts of calcium carbonate, 0.5-1.5 parts of antioxidant and nano WS20.2-1 part of superfine nickel powder, 0.4-2 parts of superfine nickel powder, wherein the total base number of the high-base-number calcium sulfonate is 350-450mgKOH/g, the base oil is mineral oil or synthetic oil, the antioxidant is diphenylamine, dioctyldiphenylamine or di-tert-butyl-p-cresol, and the nano WS2The mass ratio of the superfine nickel powder to the superfine nickel powder is 1: 2.
2. The preparation method of the high antifriction performance calcium complex sulfonate grease of claim 1, characterized by comprising the steps of:
(1) adding high-base-number calcium sulfonate, half of base oil, half of alkylbenzene sulfonic acid, calcium carbonate and water serving as solvents into a reaction kettle, heating and stirring; the heating temperature is 75-85 ℃, and the stirring time is 30-60 min;
(2) adding the rest of the base oil and the alkylbenzene sulfonic acid into a reaction kettle, heating and stirring; the temperature for heating and stirring is 85-95 ℃, and the stirring time is 30-60 min;
(3) finally adding nano WS2And superfine nickel powder, and continuously stirring; the stirring time is 30-60 min;
(4) removing the solvent under reduced pressure, and raising the temperature to 160-180 ℃ for refining; refining for 5-10 minutes;
(5) and cooling, adding an antioxidant, and further cooling to obtain the composite calcium sulfonate-based lubricating grease.
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Citations (6)
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JPH1060466A (en) * | 1996-08-22 | 1998-03-03 | Fuji Dies Kk | Self-lubricant composite material |
CN101100624A (en) * | 2007-07-18 | 2008-01-09 | 深圳先进技术研究院 | Additive for lubricating oil and preparation method thereof |
CN101113382A (en) * | 2006-07-27 | 2008-01-30 | 张念 | Formula of wheel-rack solid lubrication additive for railway traffic |
CN101935578A (en) * | 2010-10-11 | 2011-01-05 | 长沙众城石油化工有限责任公司 | Calcium sulfonate complex grease and preparation method thereof |
CN103740435A (en) * | 2014-02-11 | 2014-04-23 | 上海禾泰特种润滑技术有限公司 | Composite calcium sulfonate lubricating grease composition and preparation method thereof |
CN103820193A (en) * | 2014-02-24 | 2014-05-28 | 广东美芝制冷设备有限公司 | Lubricating oil composition and its application |
-
2018
- 2018-11-09 CN CN201811330698.8A patent/CN109370723B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH1060466A (en) * | 1996-08-22 | 1998-03-03 | Fuji Dies Kk | Self-lubricant composite material |
CN101113382A (en) * | 2006-07-27 | 2008-01-30 | 张念 | Formula of wheel-rack solid lubrication additive for railway traffic |
CN101100624A (en) * | 2007-07-18 | 2008-01-09 | 深圳先进技术研究院 | Additive for lubricating oil and preparation method thereof |
CN101935578A (en) * | 2010-10-11 | 2011-01-05 | 长沙众城石油化工有限责任公司 | Calcium sulfonate complex grease and preparation method thereof |
CN103740435A (en) * | 2014-02-11 | 2014-04-23 | 上海禾泰特种润滑技术有限公司 | Composite calcium sulfonate lubricating grease composition and preparation method thereof |
CN103820193A (en) * | 2014-02-24 | 2014-05-28 | 广东美芝制冷设备有限公司 | Lubricating oil composition and its application |
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