CN111100736B - Lubricating grease composition and preparation method thereof - Google Patents
Lubricating grease composition and preparation method thereof Download PDFInfo
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- CN111100736B CN111100736B CN201811270203.7A CN201811270203A CN111100736B CN 111100736 B CN111100736 B CN 111100736B CN 201811270203 A CN201811270203 A CN 201811270203A CN 111100736 B CN111100736 B CN 111100736B
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- grease composition
- calcium salt
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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
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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
- 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
- C10M2207/028—Overbased salts thereof
-
- 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
- C10M2207/26—Overbased carboxylic acid salts
-
- 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
- C10M2207/26—Overbased carboxylic acid salts
- C10M2207/262—Overbased carboxylic acid salts derived from hydroxy substituted aromatic acids, e.g. salicylates
-
- 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
- C10M2219/046—Overbasedsulfonic acid salts
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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 relates to the field of lubricating grease, and discloses a lubricating grease composition and a preparation method thereof. The lubricating grease composition contains base oil, a thickening agent, an organic calcium salt and an auxiliary additive, wherein the total base number of the organic calcium salt is more than or equal to 150mg KOH/g; the auxiliary additive contains organic molybdenum, thiadiazole derivatives and phosphate ester in a weight ratio of 1:0.02-50: 0.02-50. The method comprises the following steps: mixing the thickening agent and part of the base oil, heating, mixing with the rest of the base oil, cooling, and mixing with the organic calcium salt and the auxiliary additive. The lubricating grease composition disclosed by the invention has excellent wear resistance and durability, and after the lubricating grease composition runs for 8 hours in a four-ball machine method wear resistance test, the wear resistance is still about 0.4mm, and the friction coefficient is less than 0.08.
Description
Technical Field
The invention relates to the field of lubricating grease, and in particular relates to a lubricating grease composition and a preparation method thereof.
Background
With the development of economy, higher demands are made on precision, working efficiency, higher frequency of use, long life characteristics, low maintenance, and the like of mechanical equipment, and therefore, a lubricating material having better wear resistance and durability is required. If the lubrication is poor, abrasion is caused, the precision of mechanical equipment is directly influenced, the equipment is damaged, the service life is shortened, and economic loss is caused.
In order to improve the anti-wear properties of greases, it is often necessary to add anti-wear additives. Such as CN106906030A, adding dibenzyl disulfide (T322), tricresyl phosphate (T306), phosphate (T451), and phosphonitrilic amide (T3011), etc., the abrasion diameter of the grease (392N, 60min by four-ball method) is 0.42 mm; CN106497652AAdding organic molybdenum, thiophosphate and phosphate, wherein the wear diameter (392N by a four-ball method, 60min) of the lubricating grease is 0.40 mm; CN106867637A, adding 80-90% of compound lithium-based grease, 3-10% of antiwear lubricant additive, 1-5% of polytetrafluoroethylene, 1-5% of zinc oxide, 2-14% of organic molybdenum and 0.1-3% of dialkyl zinc dithiophosphate (ZDDP), and P of lubricating grease B A value of 981N; CN101889019A, adding thiadiazole poly (ether) glycol complex, molybdenum dihydrocarbyl dithiophosphate and zinc hydrocarbyl dithiophosphate, wherein the abrasion diameter (392N by four-ball method, 60min) of the lubricating grease is 0.44mm at minimum; CN1222594C, adding 0.5-5% molybdenum sulfide dialkyl dithio-carbamic acid, 0.1-5% 5, 5' -dithio-bis (1,3, 4-thiadiazole-2-thiol) and 0.1-5% triphenyl thiophosphate; CN1322104C, adding 1-4 wt% of organic molybdenum, 0.1-5 wt% of sulfur-containing additive and 0.1-5 wt% of phosphorus-containing additive; CN106590846A, adding 0.5-5% of molybdenum carbamate, zinc dithiocarbamate, sulfurized olefin, triphenyl phosphate, polytetrafluoroethylene, tricresyl phosphate, melamine cyanurate and the like.
According to the scheme provided by the above documents, the addition of the additive can improve the wear resistance of the lubricating grease, but the requirement of the wear resistance durability of the lubricating grease cannot be met, and the condition shows that the wear resistance is remarkably reduced after the lubricating grease runs for 8 hours in a four-ball machine method wear resistance test, and the lubricating grease is difficult to maintain at about 0.4 mm.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a lubricating grease composition with good wear resistance, particularly excellent wear resistance durability under a long-time condition (8h) and a preparation method thereof.
In order to achieve the above object, in a first aspect, the present invention provides a grease composition, which contains base oil, a thickener, an organic calcium salt and an auxiliary additive, wherein the total base number of the organic calcium salt is greater than or equal to 150mg KOH/g; the auxiliary additive contains organic molybdenum, thiadiazole derivatives and phosphate ester in a weight ratio of 1:0.02-50: 0.02-50.
In a second aspect, the present invention provides a method of preparing the grease composition described above, the method comprising: mixing the thickening agent and part of the base oil, heating, mixing with the rest of the base oil, cooling, and mixing with the organic calcium salt and the auxiliary additive.
In a third aspect, the present invention provides a grease composition prepared by the above method.
Through the technical scheme, the lubricating grease composition disclosed by the invention has excellent wear resistance and durability, and after the lubricating grease composition runs for 8 hours in a four-ball machine method wear resistance test, the wear resistance is still about 0.4mm (in terms of four-ball trace diameter) and the friction coefficient is less than 0.08.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In a first aspect, the lubricating grease composition provided by the invention comprises base oil, a thickening agent, an organic calcium salt and an auxiliary additive, wherein the total base number of the organic calcium salt is more than or equal to 150mg KOH/g; the auxiliary additive contains organic molybdenum, thiadiazole derivatives and phosphate ester in a weight ratio of 1:0.02-50: 0.02-50.
According to the present invention, the object of the present invention can be achieved as long as the auxiliary additive is controlled to contain the organic molybdenum, the thiadiazole derivative and the phosphate in the above-mentioned ratio, but preferably, the weight ratio between the organic molybdenum, the thiadiazole derivative and the phosphate is 1:0.15-6:0.15-6, more preferably 1:0.7-2: 0.7-2.
According to the present invention, the organomolybdenum can be various oil-soluble organomolybdenum compounds commonly used in the art, for example, molybdenum dialkyldithiophosphates, molybdenum dialkyldithiocarbamates, molybdenum amine complexes, molybdenum naphthenate, molybdenum alkylsalicylate, and the like. Preferably, the organo molybdenum is molybdenum dialkyldithiocarbamate (MoDTC) and/or molybdenum dialkyldithiophosphate (MoDTP). The number of carbon atoms of the alkyl group or cycloalkyl group in the above-mentioned organic molybdenum may be 1 to 6, for example, the alkyl group in the organic molybdenum may be methyl, ethyl, propyl, etc., and the molybdenum naphthenate may be molybdenum cyclohexanecarboxylate, etc.
According to the invention, the thiadiazole derivative is various common substances taking thiadiazole as a parent structure, in particular to substances in which sulfhydryl hydrogen on the thiadiazole is substituted (such as substituted by a group with 5-12 carbon atoms), and the thiadiazole derivative is 2, 5-di (tert-dodecyl dithio) -1,3, 4-thiadiazole and/or 2, 5-di (tert-octyl dithio) -1,3, 4-thiadiazole.
According to the invention, the phosphate comprises orthophosphoric acid ester and/or phosphorous acid ester, which means phosphoric acid and/or phosphorous acid ester derivatives, preferably, the phosphate is at least one of di-n-butyl phosphite, triphenyl phosphate and tricresyl phosphate.
According to the present invention, the content of the auxiliary additive may be conventionally selected, and preferably, the content of the auxiliary additive is 0.3 to 15 wt%, more preferably 0.9 to 5.5 wt%, based on the total weight of the grease composition.
According to the present invention, there is no particular requirement for the content of the organic calcium salt, preferably the content of the organic calcium salt is 0.1 to 5 wt.%, more preferably 1.5 to 4.5 wt.%, based on the total weight of the grease composition.
According to the invention, the organic calcium salt may be a calcium salt of a common organic acid and/or a calcium phenate, as long as the total base number thereof satisfies the above requirements. According to a preferred embodiment of the invention, the total base number of the organic calcium salt is in the range of 150-500mg KOH/g. In the present invention, the test criteria for "total base number" are: SH/T0251, "method of measuring the base number of Petroleum products (Perchloric acid potentiometry"), indicates the amount of perchloric acid required to neutralize all of the basic components in a 1g sample (organic calcium salt), expressed in milligrams of equivalent potassium hydroxide.
Wherein, the calcium salt of the organic acid can be a substance in which carboxyl hydrogen in the organic acid is replaced by calcium, for example, the organic acid can be at least one of petroleum sulfonic acid, naphthenic acid and salicylic acid; the calcium phenate may be a substance in which a hydroxyl hydrogen in phenol is substituted with calcium, and for example, the phenol may be an alkylphenol. Preferably, the organic calcium salt is at least one of calcium petroleum sulfonate (such as TBN150, TBN400), calcium alkyl phenolate (such as TBN200), calcium naphthenate (such as TBN250) and calcium salicylate (such as TBN 300).
According to the present invention, the content and kind of the base oil are not particularly limited, but preferably, the content of the base oil is 82 to 95 wt%, more preferably 83 to 93 wt%, based on the total weight of the grease composition.
According to the present invention, the base oil may be various base oils used in greases, such as mineral oils, synthetic oils (olefin oils and/or ester oils), vegetable oils, or mixtures thereof. Preferably, the base oil has a kinematic viscosity of 4 to 100mm at 100 ℃ 2 (ii) fats and oils in s. In the present invention, "kinematic viscosity" is measured with reference to GB/T265-1988.
According to the present invention, the content of the thickener is not particularly limited, but preferably, the content of the thickener is 3 to 10% by weight based on the total weight of the grease composition.
According to the invention, the thickener can be a metal soap conventionally used in the art, such as a lithium soap and/or a sodium soap, preferably the thickener is a lithium soap, in particular a lithium 12-hydroxystearate soap.
According to the present invention, the grease composition may further contain an auxiliary such as a rust inhibitor, an oiliness agent, and an antioxidant. Wherein, the antioxidant can further improve the oxidation resistance of the lubricating grease composition so as to prolong the service life of the lubricating grease composition, and can be arylamine antioxidant, such as at least one of diphenylamine, phenyl-alpha-naphthylamine and diisooctyldiphenylamine. The antioxidant may be present in an amount of 0.01 to 5 wt.%, based on the total weight of the grease composition.
The oiliness agent can further improve the lubricating property of the friction pair surface, and can be higher fatty acid (such as oleic acid and stearic acid), higher alcohol (such as stearyl alcohol), alkylamine (such as phenyltriazolyl stearyl amine) and the like. The content of the oiliness agent may be 0.01 to 4.5% by weight based on the total weight of the grease composition.
The antirust agent can further improve the rust resistance of the lubricating grease composition and can be at least one of barium petroleum sulfonate, sodium petroleum sulfonate, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid. The rust inhibitor may be contained in an amount of 0.01 to 4.5% by weight, based on the total weight of the grease composition.
In a second aspect, the present invention provides a method of preparing the grease composition comprising: mixing the thickening agent and part of the base oil, heating, mixing with the rest of the base oil, cooling, and mixing with the organic calcium salt and the auxiliary additive.
More specifically, the method comprises: mixing the thickening agent and the first part of base oil, heating to 200-210 ℃, mixing with the rest base oil, cooling to 100-110 ℃, and mixing with the organic acid calcium and auxiliary additives (and optional additives such as antirust agent, oiliness agent and antioxidant). Generally, the mixture finally obtained should also be subjected to a grinding treatment to make the material dispersion more uniform.
In a third aspect, the present invention provides a grease composition prepared by the above method.
The present invention will be described in detail below by way of examples, but the present invention is not limited thereto. In the following examples and comparative examples, the thickener used was lithium 12-hydroxystearate soap prepared by the method: adding 12-hydroxystearic acid into water, heating to melt the 12-hydroxystearic acid, gradually adding an aqueous solution of lithium hydroxide, stirring to fully react, controlling the molar ratio of the 12-hydroxystearic acid to the lithium hydroxide to be 1:1, and drying the reactant to remove water to obtain the 12-hydroxystearic acid lithium soap; other raw material manufacturers and codes used are shown in table 1 below.
TABLE 1
Examples 1 to 12 and comparative examples 1 to 14
According to the mixture ratio (weight ratio of the grease composition) shown in tables 2-4, 1/3 base oil and thickening agent are added into a reaction kettle, heating is carried out, 1/3 base oil is gradually added, the temperature is increased to 205 ℃, the rest base oil is added, the material is cooled, when the temperature is reduced to 105 ℃, organic calcium salt and auxiliary additive are gradually added, and the material is ground by three-wheel mill to uniformly disperse the material, so that a grease composition sample is prepared.
The physical and chemical properties of the grease composition samples were analyzed as follows:
penetration (0.1mm, 60 times): GB/T269-1991, the smaller the cone penetration is in 60 times of work, which indicates that the thickening capacity is stronger;
dropping point: GB/T3498-2008, the higher the dropping point, the better the high temperature performance;
abrasion resistance: SH/T0204 & ltmethod for measuring anti-wear performance of lubricating grease (four-ball method), wherein the setting condition of a four-ball tester is load 392N, and the diameters (mm) of four ball traces are measured at the running time of 1h and 8h respectively;
coefficient of friction (μ): the friction torque is determined by means of a four-ball test machine and is in accordance withThe friction coefficient was calculated by the formula (1) in which T is the friction torque, P is the axial test force (392N), and R is the radius of the steel ball (6.35 mm).
The results are shown in tables 2-4.
TABLE 2
TABLE 3
TABLE 4
Comparative example 15
Grease compositions were prepared according to the method of example 1 except that the organo molybdenum was replaced with zinc dithiocarbamate (VanlubeAZ, available from Vanderbilt) and the results of physical and chemical property analyses are shown in Table 5.
Comparative example 16
Grease compositions were prepared according to the method of example 1, except that the thiadiazole derivative was replaced with dibenzyl disulfide, and the results of physical and chemical property analyses are shown in table 5.
Comparative example 17
A grease composition was prepared according to the method of example 1, except that the phosphate was replaced with zinc dibutyldithiophosphate and the results of the physical and chemical property analyses are shown in Table 5.
Comparative example 18
Grease compositions were prepared according to the method of example 4 except that the organic calcium salt was replaced with barium petroleum sulfonate (available from Nanjing Runkou chemical), and the results of physical and chemical property analysis are shown in Table 5.
TABLE 5
As can be seen from the above examples and comparative examples, the present invention significantly improves the antiwear durability of a grease composition by compounding specific kinds of ingredients in specific proportions, and only compounding the respective components in the present application can effectively improve the antiwear durability.
Further experiments have shown that the grease composition of the present invention exhibits superior anti-wear durability compared to prior grease compositions (such as the individual greases mentioned in the background section), enabling the four-ball trace diameter to be maintained at around 0.4mm even in an anti-wear performance test run of 8 h.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are all within the protection scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention can be made, and the same should be considered as the disclosure of the present invention as long as the idea of the present invention is not violated.
Claims (10)
1. The lubricating grease composition is characterized by comprising base oil, a thickening agent, organic calcium salt and an auxiliary additive, wherein the thickening agent is lithium soap; the total base number of the organic calcium salt is more than or equal to 150mg KOH/g; the auxiliary additive contains organic molybdenum, thiadiazole derivatives and phosphate ester in a weight ratio of 1:0.7-50: 0.7-50; based on the total weight of the grease composition, the content of the organic calcium salt is 0.1-5 wt%, and the content of the auxiliary additive is 0.3-15 wt%.
2. Grease composition according to claim 1, wherein the weight ratio between the organomolybdenum, the thiadiazole derivative and the phosphate ester is 1:0.7-2: 0.7-2.
3. A grease composition according to claim 1 or 2, wherein the organomolybdenum is molybdenum dialkyldithiocarbamate and/or molybdenum dialkyldithiophosphate;
and/or the thiadiazole derivative is 2, 5-di (tert-dodecyl-dithio) -1,3, 4-thiadiazole and/or 2, 5-di (tert-octyl-dithio) -1,3, 4-thiadiazole;
and/or the phosphate ester is at least one of di-n-butyl phosphite, triphenyl phosphate and tricresyl phosphate.
4. Grease composition according to claim 1 or 2, wherein the auxiliary additive is present in an amount of 0.9 to 5.5 wt.%, based on the total weight of the grease composition.
5. Grease composition according to claim 1 or 2, wherein the organic calcium salt is present in an amount of 1.5-4.5 wt.%, based on the total weight of the grease composition.
6. Grease composition according to claim 1, wherein the organic calcium salt is at least one of calcium petroleum sulfonate, calcium alkyl phenate, calcium naphthenate and calcium salicylate.
7. Grease composition according to claim 1, wherein the base oil is present in an amount of 82-95 wt.%, based on the total weight of the grease composition; the content of the thickening agent is 3-10 wt%.
8. A grease composition according to claim 1 or 7, wherein the base oil has a kinematic viscosity at 100 ℃ of 4-100mm 2 /s。
9. A method of preparing a grease composition according to any one of claims 1-8, characterized in that the method comprises: mixing the thickening agent with part of the base oil, heating, mixing with the rest base oil, cooling, and mixing with the organic calcium salt and the auxiliary additive.
10. A grease composition made by the process of claim 9.
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WO2004003117A1 (en) * | 2002-06-28 | 2004-01-08 | Nippon Oil Corporation | Lubricating oil composition |
JP4520756B2 (en) * | 2004-02-26 | 2010-08-11 | 新日本石油株式会社 | Grease composition for constant velocity joints |
JP5219834B2 (en) * | 2005-12-15 | 2013-06-26 | ザ ルブリゾル コーポレイション | Lubricant composition for final reduction shaft |
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JP2013018857A (en) * | 2011-07-11 | 2013-01-31 | Mitsuba Corp | Lubricating grease composition for vehicle electrical component |
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