CN111139119A - Automobile constant velocity universal joint outer ball cage lubricating grease composition and preparation method thereof - Google Patents

Automobile constant velocity universal joint outer ball cage lubricating grease composition and preparation method thereof Download PDF

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Publication number
CN111139119A
CN111139119A CN202010002213.3A CN202010002213A CN111139119A CN 111139119 A CN111139119 A CN 111139119A CN 202010002213 A CN202010002213 A CN 202010002213A CN 111139119 A CN111139119 A CN 111139119A
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grease composition
constant velocity
ball cage
outer ball
lubricating grease
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CN111139119B (en
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韩占伟
张广辽
张晓凯
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China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating 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
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/065Sulfides; Selenides; Tellurides
    • C10M2201/066Molybdenum sulfide
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/106Naphthenic fractions
    • C10M2203/1065Naphthenic fractions used as base material
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/0206Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers used as base material
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/16Paraffin waxes; Petrolatum, e.g. slack wax
    • C10M2205/163Paraffin waxes; Petrolatum, e.g. slack wax used as base material
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/023Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/026Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/127Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic
    • C10M2207/1276Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic used as thickening agent
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/128Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
    • C10M2207/1285Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/16Naphthenic acids
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    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064Di- and triaryl amines
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    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22Heterocyclic nitrogen compounds
    • C10M2215/223Five-membered rings containing nitrogen and carbon only
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04Phosphate esters
    • C10M2223/045Metal containing thio derivatives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2227/00Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/06Organic compounds derived from inorganic acids or metal salts
    • C10M2227/061Esters derived from boron

Abstract

The invention relates to the technical field of lubricating grease, and particularly relates to an automobile constant velocity universal joint outer ball cage lubricating grease composition and a preparation method thereof. The lubricating grease composition for the outer ball cage of the constant velocity universal joint of the automobile comprises base oil, a thickening agent, an extreme pressure antiwear agent and an antioxidant; wherein, the using amount of the thickening agent is 5.0-20.0% based on the total mass of the lubricating grease composition; the mass ratio of the thickening agent to the extreme pressure antiwear agent to the antioxidant is 5.0-20.0: 0.5-5.0: 0.5-3.0. The lubricating grease for the outer ball cage of the constant velocity universal joint of the automobile has outstanding extreme pressure wear resistance, rust resistance and mechanical stability, is long in service life, has a use temperature range of-40-160 ℃, not only guarantees the use requirement at a low temperature, but also keeps good lubricating property at a high temperature, avoids loss, can provide more reliable and comprehensive protection for use parts, and has a good application prospect.

Description

Automobile constant velocity universal joint outer ball cage lubricating grease composition and preparation method thereof
Technical Field
The invention relates to the technical field of lubricating grease, and particularly relates to an automobile constant velocity universal joint outer ball cage lubricating grease composition and a preparation method thereof.
Background
Automobiles have gone past one hundred years of weather since their birth since the last century. With the rapid development of modern society, people increasingly pay more attention to environmental problems, the awareness of environmental protection is gradually deepened, and the requirements on the performance, the environmental protection and the like of automobiles are more and more strict.
The constant velocity universal joint (CVJ) of the automobile is an important transmission part for connecting the gearbox and wheels of the automobile, two CVJs are connected with a rigid shaft to form a transmission shaft of the automobile, and power generated by an engine is transmitted to driving wheels of the automobile in an equiangular velocity mode through the transmission shaft to drive a car to run at a high speed. The constant velocity joint on the wheel side generally employs a birfield joint that allows the change in the pinch angle of the drive shaft. The rzeppa constant velocity universal joint can move or not according to the axial direction of the universal joint, and can be simply divided into a fixed rzeppa universal joint (RF joint) and a telescopic rzeppa universal joint (VL joint), and a telescopic rubber sheath is arranged outside the rzeppa constant velocity universal joint. Structurally, the fixed ball cage universal joint has inner surface connected to the transmission shaft via inner spline, outer surface with arc notch as the inner rolling way of the steel ball and outer rolling way on the inner surface of the spherical shell. The star-shaped sleeve and the spherical shell are assembled to form a raceway, and the steel balls are positioned in the same plane by a retainer (ball cage). The power is transmitted by the transmission shaft through the steel ball and the spherical shell. The universal joint used in the automobile is similar to a joint of a human body, and allows an included angle between connected parts to be changed within a certain range so as to meet the requirement of angle change caused by up-down jumping in the automobile driving process. The operation structure and the motion principle of the CVJ are very complex, the CVJ bears complex rolling and sliding reciprocating motion in the operation process during the running process of an automobile, particularly, along with the increase of the installation angle and the operation speed of the CVJ in recent years, the temperature of the whole CVJ can be increased if the bearing runs unsmoothly, so that the CVJ cannot be fully lubricated in the motion, the rolling bodies, the inner and outer roller paths can be scratched, the roller pins are cracked and the like, and in serious cases, the running safety of the automobile is directly damaged, so that the lubricating grease for the CVJ is lubricating grease with special performance, and besides the lubricating performance of common lubricating grease, the lubricating grease also has excellent extreme pressure wear resistance, wear resistance and certain high and low temperature resistance. In the prior constant velocity universal joint outer ball cage lubricating grease, a mode of adding a solid extreme pressure anti-wear agent is usually adopted for solving the problem of insufficient extreme pressure anti-wear performance, and as the ambient temperature is likely to generate a low temperature condition of-40 ℃ in winter, the addition of the solid extreme pressure anti-wear agent can increase the consistency of the lubricating grease, deteriorate the flow performance at low temperature, lead to untimely oil film supplement, cause the contact surface to be scratched, cause serious abrasion and the like.
CN101659897A provides lubricating grease for automobile constant velocity universal joints, which adopts a lithium-based thickener, and increases the extreme pressure wear resistance by increasing the content of calcium carbonate to replace molybdenum disulfide, but the use temperature of the lithium-based lubricating grease is lower, and the high temperature requirement of the current harsh CVJ outer ball cage on the lubricating grease can not be met. CN1321733A provides a lubricating grease for constant velocity universal joints and a preparation method thereof, wherein mineral base oil and a composite lithium calcium base thickening agent are adopted, and molybdenum disulfide, molybdenum dialkyl dithiocarbamate and the like are used for improving the extreme pressure abrasion resistance, but the low temperature performance of the mineral base oil is poor, and the addition amount of the molybdenum disulfide is large, so that the lubricating grease has extremely poor flowability at the low temperature of-40 ℃ and cannot play a lubricating role.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides an automobile constant velocity universal joint outer ball cage lubricating grease composition and a preparation method thereof. The lubricating grease for the outer ball cage of the constant velocity universal joint of the automobile has outstanding extreme pressure wear resistance, rust resistance and mechanical stability and long service life, the use temperature range is-40-160 ℃, the use requirement under low temperature is ensured, the good lubricating property is kept under high temperature, and the loss is avoided.
In order to achieve the above object, in the grease composition for the outer ball cage of the constant velocity universal joint of an automobile of the present invention, a base oil, a thickener, an extreme pressure anti-wear agent, and an antioxidant are included;
the kinematic viscosity at 40 ℃ of the base oil is 60-220mm2S; the thickening agent is a composite lithium-calcium soap-based thickening agent; the extreme pressure antiwear agent is selected from one or more of molybdenum disulfide, zinc dialkyl dithiophosphate, calcium carbonate, antimony dialkyl dithiophosphate and boric acid ester; the antioxidant is an amine antioxidant and/or a phenol antioxidant;
wherein, the using amount of the thickening agent is 5.0-20.0% based on the total mass of the lubricating grease composition; the mass ratio of the thickening agent to the extreme pressure antiwear agent to the antioxidant is 5.0-20.0: 0.5-5.0: 0.5-3.0; preferably 8.0 to 15.0: 0.5-3.5: 0.5-2.5.
In the technical scheme, the base oil can meet the compatibility index of the lubricating grease on the outer ball cage sealing material, and the thickening agent, the extreme pressure antiwear agent and the antioxidant are specifically selected and proportioned, so that a good protective film is formed on the metal surface in a synergistic manner, the intermetallic wear is reduced, the service life of the lubricating grease is prolonged, and the lubricating requirement of the automobile CVJ outer ball cage is met. As a preferred scheme of the invention, the thickening agent is prepared by taking 12-hydroxystearic acid, dibasic acid, lithium hydroxide and calcium hydroxide as raw materials; preferably, the dibasic acid is one or more of sebacic acid, adipic acid and azelaic acid.
Preferably, when the mass ratio of the 12-hydroxystearic acid to the dibasic acid is 7:1 to 1:1, the mechanical stability of the grease can be further improved, and the change value of the working cone penetration is reduced.
Preferably, the mass ratio of the lithium hydroxide to the calcium hydroxide is 1:1 to 10: 1.
In a preferable embodiment of the invention, the amine antioxidant is one or two selected from diphenylamine, alkylated diphenylamine, naphthylamine and p-phenylenediamine, and the phenolic antioxidant is 2, 6-di-tert-butyl-p-cresol or α -naphthol.
As a preferred embodiment of the present invention, the base oil is PAO synthetic oil; or, a mixture of PAO synthetic oil and at least one selected from paraffin-based mineral oil, naphthenic mineral oil; preferably the viscosity index of the base oil is not less than 100; preferably, based on the mass of the base oil, when the content of the PAO synthetic oil is more than or equal to 30%, other properties can be ensured, and simultaneously, the low-temperature performance of the oil product is considered.
In a preferred embodiment of the present invention, the grease composition further comprises 0.01 to 3.0% (preferably 0.01 to 1.0%) of an anti-rust preservative based on the total mass of the grease composition, wherein the anti-rust preservative is a benzotriazole derivative and/or a naphthenate, preferably benzotriazole and/or zinc naphthenate.
In a preferred embodiment of the present invention, the grease composition for the outer ball cage of the constant velocity universal joint of the automobile comprises the following components by weight:
Figure BDA0002353881780000041
those skilled in the art can combine the above preferred embodiments to obtain preferred embodiments of the present invention, as is well understood in the art.
The invention further provides a preparation method of the lubricating grease composition for the outer ball cage of the automobile constant velocity universal joint, which comprises the following steps:
adding 30-50% of base oil and all 12-hydroxystearic acid into a reaction kettle, heating to 80-90 ℃, adding part of lithium hydroxide solution and all calcium hydroxide solution, and reacting for 30-60 min; adding dibasic acid at 90-100 deg.c; after stirring for 40-50 minutes, beginning to dropwise add the rest lithium hydroxide solution at the temperature of 95-100 ℃; after the reaction is finished, heating to 130-140 ℃, and keeping the temperature for 60-90 min; heating to 150-;
preferably, when the extreme pressure antiwear agent is added, the antirust preservative is added together.
The method further comprises the steps of dispersing, grinding, canning and the like after the raw material mixing is finished, and is not further limited.
Compared with the similar lubricating grease product, the automobile constant velocity universal joint outer ball cage lubricating grease provided by the invention at least has the following advantages:
1) the lubricating grease disclosed by the invention has good extreme pressure performance, and the PD can reach 3923N which is obviously higher than 2452N of the existing index.
2) The lubricating grease disclosed by the invention has good wear resistance, and the minimum diameter of a wear scar can reach 0.4mm by adopting an SH/T0204 method for testing.
3) The lubricating grease prepared by the invention has good antirust performance, and all bearings have no rust when tested by using a GB/T5018 method.
4) The lubricating grease prepared by the invention has good wear resistance and friction reduction performance, and the friction coefficient is 0.09-0.20 when tested by using an ASTM5707 method.
5) The lubricating grease disclosed by the invention has lower bearing operating temperature and can meet the use requirement of-40 ℃.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Example 1
The embodiment provides an outer ball cage lubricating grease composition of an automobile constant velocity universal joint, which comprises the following components:
a thickening agent: 280.0g, wherein, 12-hydroxystearic acid: the mass ratio of azelaic acid is 6:1, lithium hydroxide: the mass ratio of the calcium hydroxide is 9: 1;
base oil: 2400g (PAO synthetic oil: 100%, base oil kinematic viscosity at 40 ℃ C.: 114.5 mm)2(ii)/s, viscosity index 129);
extreme pressure antiwear agent: molybdenum disulfide: 53.6 g; 53.6g of zinc dialkyl dithiophosphate and 26.8g of calcium carbonate;
antioxidant: 13.4g of 2, 6-di-tert-butyl-p-cresol and 13.4g of alkylated diphenylamine;
antirust and antiseptic: 26.8g of zinc naphthenate.
The embodiment further provides a preparation method of the automobile constant velocity universal joint outer ball cage lubricating grease composition, which specifically comprises the following steps:
1) 960g of base oil and all 12-hydroxystearic acid are added into a reaction kettle, the temperature is raised to 85 ℃, and a proper amount of lithium hydroxide solution and all calcium hydroxide solution are added to start the reaction for 1 hour. Adding dibasic acid at 90 deg.c; after stirring for 45 minutes, beginning to dropwise add the residual lithium hydroxide solution when the temperature is 98 ℃;
2) after the reaction is finished, stirring and heating to 135 ℃, keeping the temperature for 70min, heating to 170 ℃, adding 480g of base oil and all antioxidants, continuing heating to 210 ℃, adding the rest base oil for cooling, cooling to 80 ℃, adding the extreme pressure antiwear agent and the antirust preservative, stirring uniformly, dispersing and grinding by post-treatment equipment, and then canning the finished product.
Example 2
The embodiment provides an outer ball cage lubricating grease composition of an automobile constant velocity universal joint, which comprises the following components:
a thickening agent: 320g, wherein the ratio of 12-hydroxystearic acid: the mass ratio of azelaic acid is 3:1, lithium hydroxide: the mass ratio of the calcium hydroxide is 3: 1;
base oil: 2600g (wherein the naphthenic base mineral oil is 70%, the PAO synthetic oil is 30%, and the base oil has a kinematic viscosity at 40 ℃ of 115.5mm2(ii)/s, viscosity index of 122);
extreme pressure antiwear agent: molybdenum disulfide: 29.2 g; 29.2g of zinc dialkyldithiophosphate; 29.2g of calcium carbonate;
antioxidant: 14.6g of alkylated diphenylamine, 14.6g of 2, 6-di-tert-butyl-p-cresol;
antirust and antiseptic: 1.5g of benzotriazole and 14.6g of zinc naphthenate.
The embodiment further provides a preparation method of the automobile constant velocity universal joint outer ball cage lubricating grease composition, which specifically comprises the following steps:
1) 1040g of base oil and all of 12-hydroxystearic acid are added into a reaction kettle, the temperature is raised to 87 ℃, and a proper amount of lithium hydroxide solution and all of calcium hydroxide solution are added to start the reaction for 1 hour. Adding dibasic acid at 92 deg.c; after stirring for 40 minutes, beginning to dropwise add the rest lithium hydroxide solution when the temperature is 95 ℃;
2) after the reaction is finished, stirring and heating to 130 ℃, keeping the temperature for 90min, heating to 165 ℃, adding 580g of base oil and all antioxidants, continuing heating to 208 ℃, adding the rest base oil for cooling, cooling to 80 ℃, adding the extreme pressure antiwear agent and the antirust preservative, stirring uniformly, dispersing and grinding by post-treatment equipment, and then canning the finished product.
Example 3
The embodiment provides an outer ball cage lubricating grease composition of an automobile constant velocity universal joint, which comprises the following components:
a thickening agent: 300g, wherein 12-hydroxystearic acid: the mass ratio of azelaic acid is 2:1, lithium hydroxide: the mass ratio of the calcium hydroxide is 4: 1;
base oil: 2500g (wherein paraffin base mineral oil 20%, PAO synthetic oil 80%, base oil 40 ℃ kinematic viscosity: 100.8 mm)2(ii)/s, viscosity index of 125);
extreme pressure antiwear agent: molybdenum disulfide: 42g of the total weight of the mixture; 28g of borate; 42g of phosphate ester;
antioxidant: 42g of alkylated diphenylamine;
antirust and antiseptic: 42g of zinc naphthenate.
The embodiment further provides a preparation method of the automobile constant velocity universal joint outer ball cage lubricating grease composition, which specifically comprises the following steps:
1) 1000g of base oil and all 12-hydroxystearic acid are added into a reaction kettle, the temperature is raised to 80 ℃, and a proper amount of lithium hydroxide solution and all calcium hydroxide solution are added to start reaction for 1 hour. Adding dibasic acid at 95 deg.c; after stirring for 45 minutes, beginning to dropwise add the residual lithium hydroxide solution when the temperature is 99 ℃;
2) after the reaction is finished, stirring and heating to 132 ℃, keeping the temperature for 70min, heating to 180 ℃, adding 500g of base oil and all antioxidants, continuously heating to 200 ℃, adding the rest base oil for cooling, cooling to 80 ℃, adding the extreme pressure antiwear agent and the antirust preservative, stirring uniformly, dispersing and grinding by post-treatment equipment, and then canning the finished product.
Example 4
The embodiment provides an outer ball cage lubricating grease composition of an automobile constant velocity universal joint, which comprises the following components:
a thickening agent: 300g, wherein 12-hydroxystearic acid: the mass ratio of azelaic acid is 5:1, lithium hydroxide: the mass ratio of the calcium hydroxide is 9: 1;
base oil: 2500g (wherein the naphthenic base mineral oil is 20%, the paraffin base mineral oil is 10%, the PAO synthetic oil is 70%, and the base oil has a kinematic viscosity at 40 ℃ of 110.1mm2(ii)/s, viscosity index 113);
extreme pressure antiwear agent: molybdenum disulfide: 42g, 28g of calcium carbonate, 42g of zinc dialkyl dithiophosphate and 14g of borate;
antioxidant: 28g of diphenylamine, 28g of 2, 6-di-tert-butyl-p-cresol;
antirust and antiseptic: 2.8g of benzotriazole and 28g of zinc naphthenate.
The embodiment further provides a preparation method of the automobile constant velocity universal joint outer ball cage lubricating grease composition, which specifically comprises the following steps:
1) 1000g of base oil and all 12-hydroxystearic acid are added into a reaction kettle, the temperature is raised to 80 ℃, and a proper amount of lithium hydroxide solution and all calcium hydroxide solution are added to start reaction for 1 hour. Adding dibasic acid at 100 deg.c; after stirring for 50 minutes, beginning to dropwise add the rest lithium hydroxide solution when the temperature is 100 ℃;
2) after the reaction is finished, stirring and heating to 140 ℃, keeping the temperature for 60min, heating to 160 ℃, adding 500g of base oil and all antioxidants, continuing heating to 210 ℃, adding the rest base oil for cooling, cooling to 80 ℃, adding the extreme pressure antiwear agent and the antirust preservative, stirring uniformly, dispersing and grinding by post-treatment equipment, and then canning the finished product.
Example 5
The embodiment provides an outer ball cage lubricating grease composition of an automobile constant velocity universal joint, which comprises the following components:
a thickening agent: 240g, wherein 12-hydroxystearic acid: the mass ratio of azelaic acid is 7:1, lithium hydroxide: the mass ratio of the calcium hydroxide is 5: 1;
base oil: 2000g (wherein the naphthenic base mineral oil is 35%, the paraffin base mineral oil is 35%, the PAO synthetic oil is 30%, and the kinematic viscosity of the base oil at 40 ℃ is 100.8mm2(ii) a viscosity index of 106);
extreme pressure antiwear agent: molybdenum disulfide: 22.4 g; 22.4g of calcium carbonate, 11.2g of phosphate and 11.2g of antimony dialkyl dithiophosphate;
antioxidant: 33.6g of 2, 6-di-tert-butyl-p-cresol;
antirust and antiseptic: 3.36g of benzotriazole.
The embodiment further provides a preparation method of the automobile constant velocity universal joint outer ball cage lubricating grease composition, which specifically comprises the following steps:
1) adding 800g of base oil and all 12-hydroxystearic acid into a reaction kettle, heating to 90 ℃, adding a proper amount of lithium hydroxide solution and all calcium hydroxide solution, and starting to react for 1 hour. Adding dibasic acid at 98 deg.c; after stirring for 45 minutes, beginning to dropwise add the residual lithium hydroxide solution when the temperature is 99 ℃;
2) after the reaction is finished, stirring and heating to 131 ℃, keeping the temperature for 60min, heating to 175 ℃, adding 569g of base oil and all antioxidants, continuing heating to 209 ℃, adding the rest base oil for cooling, cooling to 80 ℃, adding the extreme pressure antiwear agent and the antirust preservative, stirring uniformly, dispersing and grinding by post-treatment equipment, and then canning the finished product.
Comparative example 1
This comparative example provides an outer ball cage grease composition for an automobile constant velocity joint, which is different from example 4 in the composition of the extreme pressure antiwear agent.
Specifically, the extreme pressure antiwear agent comprises the following components: molybdenum disulfide: 42g of the total weight of the mixture; 42g of zinc dialkyldithiophosphate; 28g of borate ester.
The preparation method of the grease composition for the outer ball cage of the constant velocity universal joint of the automobile is the same as that of example 4.
Comparative example 2
This comparative example provides an outer ball cage grease composition for an automobile constant velocity joint, which is mainly different from example 4 in the composition ratio of the thickener.
Specifically, the thickener consists of: 12-hydroxystearic acid: the mass ratio of azelaic acid is 8: 1. The preparation method of the grease composition for the outer ball cage of the constant velocity universal joint of the automobile is the same as that of example 4.
Experimental example 1
The greases obtained in examples 1 to 5 and comparative examples 1 to 2 were subjected to performance tests (see table 1 for test results).
Table 1 grease performance test results
Figure BDA0002353881780000091
Figure BDA0002353881780000101
As can be seen from the data in table 1, the greases prepared in examples 1 to 5 of the present invention all exhibited excellent mechanical stability, good extreme pressure wear resistance, good low temperature performance, rust prevention performance, and excellent friction reduction performance. This is particularly true: compared with the comparative example 1, the extreme pressure antiwear performance of the example 4 is better than that of the comparative example 1; example 4 compared to comparative example 2, the shear resistance is significantly better than comparative example 2. Completely meets the requirements of the CVJ outer ball cage of the automobile on lubricating grease and the working condition of field operation. The grease for the constant velocity universal joint outer ball cage prepared by the invention has excellent mechanical stability and high and low temperature performance, ensures the normal and stable operation of the universal joint in the environment of different climates, different regions and different seasons, has excellent extreme pressure wear resistance, and meets the use requirement of the outer ball cage under the high load condition. The high-performance anti-rust universal joint has good anti-rust performance, protects the outer ball cage from being eroded by the external environment, and ensures the maximum transmission efficiency of the universal joint due to excellent antifriction performance. The invention can provide more reliable and comprehensive protection for the use part and has good application prospect.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. The lubricating grease composition for the outer ball cage of the constant velocity universal joint of the automobile comprises base oil, a thickening agent and an extreme pressure antiwear agent, and is characterized by also comprising an antioxidant;
the kinematic viscosity at 40 ℃ of the base oil is 60-220mm2S; the thickening agent is a composite lithium-calcium soap-based thickening agent; the extreme pressure antiwear agent is selected from one or more of molybdenum disulfide, zinc dialkyl dithiophosphate, calcium carbonate, phosphate, antimony dialkyl dithiophosphate and boric acid ester; the antioxidant is an amine antioxidant and/or a phenol antioxidant;
wherein, the using amount of the thickening agent is 5.0-20.0% based on the total mass of the lubricating grease composition; the mass ratio of the thickening agent to the extreme pressure antiwear agent to the antioxidant is 5.0-20.0: 0.5-5.0: 0.5-3.0.
2. The grease composition for the outer ball cage of the constant velocity universal joint of the automobile according to claim 1, wherein the thickener is prepared from 12-hydroxystearic acid, a dibasic acid, lithium hydroxide and calcium hydroxide.
3. The automotive constant velocity joint outer ball cage grease composition according to claim 2, wherein the dibasic acid is one or more of sebacic acid, adipic acid, and azelaic acid.
4. The automotive constant velocity joint outer ball cage grease composition according to claim 2 or 3, characterized in that the mass ratio of the 12-hydroxystearic acid to the dibasic acid is 7:1 to 1: 1.
5. The automotive constant velocity joint outer ball cage grease composition according to any one of claims 2 to 4, characterized in that the mass ratio of the lithium hydroxide to the calcium hydroxide is from 1:1 to 10: 1.
6. The grease composition as claimed in any one of claims 1 to 5, wherein the amine antioxidant is one or two selected from diphenylamine, alkylated diphenylamine, naphthylamine and p-phenylenediamine, and the phenolic antioxidant is 2, 6-di-tert-butyl-p-cresol or α -naphthol.
7. The automotive constant velocity joint outer cage grease composition according to any one of claims 1 to 6, characterized in that the base oil is a PAO synthetic oil; or, a mixture of PAO synthetic oil and at least one selected from paraffin-based mineral oil, naphthenic mineral oil; preferably the viscosity index of the base oil is not less than 100; preferably, the content of the PAO synthetic oil is more than or equal to 30 percent based on the mass of the base oil.
8. The grease composition for the outer ball cage of the constant velocity universal joint of an automobile according to any one of claims 1 to 7, further comprising 0.01 to 3.0% of an anti-rust preservative based on the total mass of the grease composition, wherein the anti-rust preservative is a benzotriazole derivative and/or a naphthenate salt, preferably benzotriazole and/or zinc naphthenate.
9. The automotive constant velocity joint outer cage grease composition according to any one of claims 1 to 8, characterized by being composed of the following components in the following weight ratios:
Figure FDA0002353881770000021
10. the method for preparing an automotive constant velocity joint outer cage grease composition according to any one of claims 2 to 9, characterized by comprising:
adding 30-50% of base oil and all 12-hydroxystearic acid into a reaction kettle, heating to 80-90 ℃, adding part of lithium hydroxide solution and all calcium hydroxide solution, and reacting for 30-60 min; adding dibasic acid at 90-100 deg.c; after stirring for 40-50 minutes, beginning to dropwise add the rest lithium hydroxide solution at the temperature of 95-100 ℃; after the reaction is finished, heating to 130-140 ℃, and keeping the temperature for 60-90 min; heating to 150-;
preferably, when the extreme pressure antiwear agent is added, the antirust preservative is added together.
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CN113355148A (en) * 2021-05-28 2021-09-07 中国石油化工股份有限公司 Lubricant for automobile driving shaft hub bearing joint surface and preparation method thereof
CN113943597A (en) * 2021-10-28 2022-01-18 中国石油化工股份有限公司 Lubricating grease composition for new energy automobile and preparation method thereof
CN115232659A (en) * 2022-02-08 2022-10-25 中国石油化工股份有限公司 Constant velocity universal joint outer ball cage lubricating grease composition in automobile service market and preparation method thereof

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