CN113512453B - Electric automobile hub bearing lubricating grease composition and preparation method thereof - Google Patents

Electric automobile hub bearing lubricating grease composition and preparation method thereof Download PDF

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Publication number
CN113512453B
CN113512453B CN202110719048.8A CN202110719048A CN113512453B CN 113512453 B CN113512453 B CN 113512453B CN 202110719048 A CN202110719048 A CN 202110719048A CN 113512453 B CN113512453 B CN 113512453B
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hub bearing
grease composition
thickening agent
lubricating grease
automobile hub
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CN113512453A (en
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韩鹏
陈芳蕾
刘建龙
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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
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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
    • 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
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/08Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
    • C10M2209/084Acrylate; Methacrylate
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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
    • C10M2215/065Phenyl-Naphthyl amines
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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
    • C10M2217/00Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/045Polyureas; Polyurethanes
    • C10M2217/0456Polyureas; Polyurethanes used as thickening agents
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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
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    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
    • C10M2219/066Thiocarbamic type compounds
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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
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/10Inhibition of oxidation, e.g. anti-oxidants
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/26Waterproofing or water resistance
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/68Shear stability
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/02Bearings
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

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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 provides a grease composition for an electric automobile hub bearing and a preparation method thereof, wherein the grease composition for the electric automobile hub bearing comprises the following components: the lubricant comprises base oil, a thickening agent and additives, wherein the additives comprise one or more of an antioxidant, an extreme pressure anti-wear agent, an antirust agent and a tackifier; the base oil is PAO base oil, the thickening agent is an aromatic polyurea thickening agent, and the mass ratio of the base oil to the thickening agent is 70-75: 16 to 21. The lubricating grease composition for the hub bearing of the electric automobile, provided by the invention, has excellent high-temperature resistance and oxidation resistance, low starting torque performance, water-resistant and rust-proof performance, extreme pressure abrasion resistance and shear loss resistance, and can better meet the service performance requirements of the hub bearing of the electric automobile.

Description

Lubricating grease composition for hub bearing of electric automobile and preparation method of lubricating grease composition
Technical Field
The invention relates to the technical field of lubricating grease, in particular to a lubricating grease composition for an electric automobile hub bearing and a preparation method thereof.
Background
The electric automobile is a vehicle with a vehicle-mounted rechargeable battery providing a power source, has the advantages of less emission, low noise, simple and convenient maintenance and the like in the driving process, and has wide prospect. The hub bearing is one of the core parts of the electric automobile. The hub bearing of the electric automobile is developed on the basis of the traditional fuel oil wheel hub bearing technology, and a plurality of same technical characteristics exist between the two types of bearings. Therefore, the lubricating grease of the two lubricating greases has many common points in performance requirements, such as excellent high temperature resistance, oxidation resistance, low starting torque performance, water resistance, rust resistance and the like. Meanwhile, compared with the traditional fuel vehicle, the electric vehicle has the obvious characteristics of self and can meet higher performance requirements on the lubricating grease of the hub bearing, such as:
(1) the automobile hub bearing lubricating grease for the electric automobile needs to have more excellent extreme pressure anti-wear performance. The electric automobile is limited by the current battery energy density technology, the whole automobile weight is generally large, and the larger whole automobile weight means that a hub bearing needs to bear larger load, and the hub bearing lubricating grease is required to have more excellent extreme pressure abrasion resistance.
(2) The automobile hub bearing lubricating grease for the electric automobile needs to have more excellent shear loss resistance. Compared with a traditional fuel vehicle, the electric vehicle has more excellent acceleration performance, which means that the hub bearing of the electric vehicle needs to bear higher acceleration, and the lubricating grease of the hub bearing can be sheared more violently, so that the leakage is easier to occur.
In conclusion, the electric automobile also provides high service performance requirements for the hub bearing lubricating grease, including excellent high-temperature-resistant oxidation resistance, low starting torque performance, water-resistant anti-rust performance, extreme pressure anti-wear performance, anti-shear leakage performance and the like. Therefore, in order to improve the reliability of the hub bearing of the electric automobile and reduce the occurrence rate of faults, it is very important to design and research the lubricating grease meeting the performance requirements of the hub bearing of the electric automobile.
Disclosure of Invention
The invention provides a lubricating grease composition for an electric automobile hub bearing and a preparation method thereof. The aromatic polyurea lubricating grease composition applied to the hub bearing of the electric automobile is provided by optimizing the formula and the process of the lubricating grease, so that the lubricating grease has excellent comprehensive properties, and the service performance requirements of the hub bearing of the electric automobile are better met. The automobile hub bearing lubricating grease composition for the electric automobile has excellent high-temperature-resistant oxidation resistance, low starting torque performance, water-resistant anti-rust performance, extreme pressure anti-wear performance and anti-shearing leakage performance.
The invention provides a lubricating grease composition for an electric automobile hub bearing, which comprises the following components: the lubricant comprises base oil, a thickening agent and additives, wherein the additives comprise one or more of an antioxidant, an extreme pressure anti-wear agent, an antirust agent and a tackifier; the base oil is PAO base oil, the thickening agent is an aromatic polyurea thickening agent, and the mass ratio of the base oil to the thickening agent is 70-75: 16 to 21. In the invention, the adopted aromatic polyurea lubricating grease is novel lubricating grease with excellent high-temperature resistance and oxidation resistance. According to a great deal of research, when the base oil with excellent low-temperature performance is compounded with the base oil, the obtained lubricating grease can better meet the performance requirement of an electric automobile hub bearing, the base oil with excellent low-temperature performance is further screened, and especially when the PAO base oil and the aromatic polyurea thickening agent are compounded according to the ratio of 70-75: 16-21, the effects in all aspects are improved ideally.
According to the invention, on the basis of the specific requirements of the hub bearing of the electric automobile, the polyurea thickening agent and the PAO base oil are further screened. The screened addition system is adopted, so that the performance of the automobile hub bearing lubricating grease composition for the electric automobile is more excellent.
According to the automobile hub bearing lubricating grease composition for the electric automobile, provided by the invention, the polyurea thickening agent is prepared from the following components in a molar ratio of 0.5-8: 1 is preferably 2:1 with diisocyanate; preferably, the aromatic amine is aniline and/or p-toluidine; the diisocyanate is toluene diisocyanate and/or 4, 4' -diisocyanate diphenylmethane.
According to the automobile hub bearing lubricating grease composition for the electric automobile, provided by the invention, the viscosity of the PAO base oil at 40 ℃ is 80-150 mm2The pour point is less than or equal to minus 40 ℃, and the viscosity index is more than or equal to 120.
According to the invention, the additive is further optimized according to the main components and the performance requirements, and the optimized additive system is adopted, so that the automobile hub bearing lubricating grease composition for the electric automobile has more excellent comprehensive performance.
According to the automobile hub bearing lubricating grease composition for the electric automobile, the additive consists of an antioxidant, an extreme pressure anti-wear agent, an antirust agent and a tackifier; preferably, the mass ratio of the antioxidant to the extreme pressure anti-wear agent to the antirust to the tackifier is (0.9-1.0): 4.5-5.0: 1.7-2.3: 0.9 to 1.0.
According to the automobile hub bearing grease composition for the electric automobile, provided by the invention, the antioxidant is a compound mixture of di-tert-butyl p-cresol and alkyl phenyl-alpha-naphthylamine; preferably, the mass ratio of the compound of the di-tert-butyl-p-cresol and the alkyl phenyl-alpha-naphthylamine is 0.1-10: 1, preferably 1: 1; the mass of the antioxidant is 0.9-1.0% of the total mass of the composition.
According to the automobile hub bearing lubricating grease composition for the electric automobile, provided by the invention, the extreme pressure antiwear agent is one or a mixture of zinc dialkyl dithiophosphate and dialkyl dithiocarbamate; preferably, the weight of the extreme pressure antiwear agent is 4.5-5.0% of the total weight of the composition.
According to the automobile hub bearing lubricating grease composition for the electric automobile, provided by the invention, the antirust agent is barium dinonylnaphthalene sulfonate; preferably, the mass of the antirust agent is 1.7-2.3% of the total mass of the composition.
According to the automobile hub bearing lubricating grease composition for the electric automobile, provided by the invention, the tackifier is polymethacrylate; preferably, the mass of the tackifier is 0.9-1.0% of the total mass of the composition.
The invention provides a grease composition for an electric automobile hub bearing, which comprises the following components in parts by weight:
Figure BDA0003136234180000031
Figure BDA0003136234180000041
according to the invention, the preferred antioxidant is a mixture of di-tert-butyl-p-cresol and alkyl phenyl-alpha-naphthylamine in a mass ratio of 1:1, and the purity of the di-tert-butyl-p-cresol is more than or equal to 99.0%. The purity of the alkyl phenyl-alpha-naphthylamine is more than or equal to 98.0 percent. The zinc dialkyl dithiophosphate contains 8.5-10.0% of zinc, 14.0-18.0% of sulfur and 7.2-8.5% of phosphorus. The dialkyl dithiocarbamate has a sulfur content of 28.0-32.0% and a viscosity of 13.5-15.5 mm at 100 ℃2And s. Barium content in barium dinonylnaphthalene sulfonate is 6.5-10.0%, and viscosity at 100 ℃ is 60-75 mm2And(s) in the presence of a catalyst. Polymethacrylic acidThe ester preferably has a viscosity of 800-1200 mm at 100 DEG C2(ii) a molecular weight of not more than 25 ten thousand.
According to the invention, the components have more comprehensive effects. In the invention, the optimal dosage ratio of the antioxidant, the extreme pressure antiwear agent, the antirust agent and the tackifier in the additive system is 1:5:2: 1; by adopting the antioxidant additive with the dosage of 1.0 part, the lubricating grease composition has more excellent antioxidant performance. The lubricating grease composition can have more excellent extreme pressure anti-wear performance by adopting 5.0 parts of extreme pressure anti-wear agent. The 2.0 parts of antirust agent is adopted, so that the lubricating grease composition has more excellent water-resistant antirust performance. In the invention, the tackifier with the use amount of 1.0 part can enable the lubricating grease composition to have more excellent adhesion performance.
The invention also provides a preparation method of the lubricating grease composition for the hub bearing of the electric automobile, which comprises the following steps: mixing the polyurea thickening agent with PAO base oil, and then mixing with an additive; preferably, the aromatic polyurea lubricating grease is prepared by adopting a prefabricated thickening agent method; more preferably, it comprises: respectively dissolving diisocyanate and aromatic amine in an organic solvent N, N-dimethylformamide, and stirring to obtain an isocyanate solution and an aromatic amine solution; mixing and reacting the isocyanate solution with the aromatic amine solution; then filtering, drying and grinding are carried out to obtain the aromatic polyurea thickening agent; mixing the aromatic polyurea thickening agent and the PAO base oil, and heating to 140-160 ℃ to form a lubricating grease precursor; cooling the lubricating grease precursor to 100-120 ℃, and mixing the lubricating grease precursor with the additive; and then continuously cooling, homogenizing, degassing and filtering to obtain the automobile hub bearing lubricating grease composition for the electric automobile. According to the invention, a preparation method for producing the aromatic polyurea thickening agent by a prefabricated thickening agent method is provided for a formula of the lubricating grease composition, the problem that isocyanate and aromatic amine are not easy to completely react in the production process of the aromatic polyurea lubricating grease is solved, the preparation method is simple and convenient to operate, and the lubricating grease is convenient to popularize and apply. According to the invention, the organic solvent N, N-dimethylformamide is used as a solvent in the reaction process of isocyanate and aromatic amine, so that reactants can be dispersed in the solvent more fully, and a polyurea thickening agent generated in the reaction process can be separated out from the solvent immediately without hindering the further reaction, thereby ensuring that the isocyanate and the aromatic amine can participate in the reaction more fully.
According to the invention, the high-temperature resistance and oxidation resistance of the lubricating grease are the most key service performance of the hub bearing lubricating grease through bench tests and practical experience of application for many years. Compared with the traditional soap-based lubricating grease, the polyurea lubricating grease is a novel lubricating grease with more excellent high-temperature resistance and oxidation resistance, and has more excellent service performance. Among different polyurea lubricating grease systems, the aromatic polyurea lubricating grease has the most excellent high-temperature resistance and oxidation resistance. Furthermore, the thickening agent used by the aromatic polyurea lubricating grease is obtained by reacting isocyanate and aromatic amine according to a ratio, and the reaction speed is very high. In the traditional polyurea production technology, isocyanate and aromatic amine are reacted in base oil, and a polyurea thickening agent generated in the reaction process is easily wrapped outside a reactant to hinder the reaction, so that the reactant cannot completely participate in the reaction, and the reactant is remained in the lubricating grease. Both isocyanates and aromatic amines are highly toxic and corrosive, and their residues in the grease affect the safety of the grease product. The aromatic polyurea lubricating grease is produced by adopting a prefabricated thickening agent method, so that reactants can fully react according to a ratio, the residue of the reactants is avoided, and the safety of the lubricating grease is improved.
The invention has the beneficial effects that: aiming at the hub bearing of the electric automobile, the invention provides lubricating grease with excellent high-temperature resistance and oxidation resistance, low starting moment performance, water-resistant and rust-proof performance, extreme pressure abrasion resistance and shear loss resistance, and meets the use performance requirement of the hub bearing of the electric automobile. The invention provides a preparation method for producing an aromatic polyurea thickening agent by a prefabricated thickening agent method aiming at a lubricating grease composition formula, solves the problem that isocyanate and aromatic amine are difficult to completely react in the production process of aromatic polyurea lubricating grease, is simple and convenient to operate, and facilitates popularization and application of the lubricating grease.
Detailed Description
To make the objects, technical solutions and advantages of the present invention clearer and more complete, the technical solutions of the present invention will be described below clearly, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present 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 instruments and the like are conventional products which are purchased by normal distributors and are not indicated by manufacturers. The process is conventional unless otherwise specified, and the starting materials are commercially available from the open literature. 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.
In the following embodiments of the invention, the antioxidant is a mixture of di-tert-butyl-p-cresol and alkyl phenyl-alpha-naphthylamine in a mass ratio of 1:1, and the purity of the di-tert-butyl-p-cresol is more than or equal to 99.0%. The purity of the alkyl phenyl-alpha-naphthylamine is more than or equal to 98.0 percent. The zinc dialkyl dithiophosphate contains 8.5-10.0% of zinc, 14.0-18.0% of sulfur and 7.2-8.5% of phosphorus. The dialkyl dithiocarbamate has a sulfur content of 28.0-32.0% and a viscosity of 13.5-15.5 mm at 100 ℃2And s. Barium content in barium dinonylnaphthalenesulfonate is 6.5-10.0%, and viscosity at 100 ℃ is 60-75 mm2And s. The preferable viscosity of the polymethacrylate at 100 ℃ is 800-1200 mm2(ii) a molecular weight of not more than 25 ten thousand.
Example 1
The embodiment provides a lubricating grease composition for an electric automobile hub bearing, which comprises the following preparation methods: 73.6g of toluene diisocyanate and 86.4g of aniline were dissolved in N, N-dimethylformamide as an organic solvent to form an isocyanate solution and an aniline solution, respectively. The aniline solution was added to the toluene diisocyanate solution, mixed and reacted with thorough stirring. And filtering and collecting the polyurea thickening agent, drying and grinding the polyurea thickening agent into powder. And mixing the polyurea thickening agent powder with 750g of PAO base oil, fully stirring and heating to 140-160 ℃ to form lubricating grease. The temperature of the lubricating grease is reduced to 100 ℃ and 120 ℃, 5g of di-tert-butyl-p-cresol, 5g of alkyl phenyl-alpha-naphthylamine, 50g of zinc dialkyl dithiophosphate, 20g of barium dinonyl naphthalene sulfonate and 10g of polymethacrylate are added and stirred uniformly. And continuously cooling to normal temperature, homogenizing, degassing and filtering to obtain the finished lubricating grease.
Example 2
The embodiment provides a lubricating grease composition for an electric automobile hub bearing, which comprises the following preparation methods: 32.5g of toluene diisocyanate and 51.2g of 4, 4' -diisocyanate diphenylmethane were dissolved in an organic solvent of N, N-dimethylformamide to form an isocyanate solution. 76.3g of aniline was dissolved in N, N-dimethylformamide as an organic solvent to form an aniline solution. The aniline solution was added to the isocyanate solution, mixed and reacted with thorough stirring. And filtering and collecting the polyurea thickening agent, drying and grinding the polyurea thickening agent into powder. The polyurea thickening agent powder is mixed with 750g of PAO base oil, fully stirred and heated to 140 ℃ and 160 ℃ to form the lubricating grease. The temperature of the lubricating grease is reduced to 100 ℃ and 120 ℃, 5g of di-tert-butyl-p-cresol, 5g of alkyl phenyl-alpha-naphthylamine, 50g of dialkyl dithiocarbamate, 20g of barium dinonyl naphthalene sulfonate and 10g of polymethacrylate are added and stirred uniformly. And continuously cooling to normal temperature, homogenizing, degassing and filtering to obtain the finished product of the lubricating grease.
Example 3
The embodiment provides a lubricating grease composition for an electric automobile hub bearing, which comprises the following preparation methods: 97.0g of 4, 4' -diisocyanate diphenylmethane and 83.0g of p-toluidine were dissolved in an organic solvent, N-dimethylformamide, respectively, to form an isocyanate solution and a p-toluidine solution. The p-toluidine solution was added to the isocyanate solution, mixed and reacted with thorough stirring. And filtering and collecting the polyurea thickening agent, drying and grinding the polyurea thickening agent into powder. The polyurea thickening agent powder is mixed with 730g of PAO base oil, fully stirred and heated to 140 ℃ and 160 ℃ to form the lubricating grease. The temperature of the lubricating grease is reduced to 100 ℃ and 120 ℃, 5g of di-tert-butyl-p-cresol, 5g of alkyl phenyl-alpha-naphthylamine, 20g of zinc dialkyl dithiophosphate, 30g of dialkyl dithiocarbamate, 20g of barium dinonyl naphthalene sulfonate and 10g of polymethacrylate are added and stirred uniformly. And continuously cooling to normal temperature, homogenizing, degassing and filtering to obtain the finished product of the lubricating grease.
Example 4
The embodiment provides a lubricating grease composition for an electric automobile hub bearing, which comprises the following preparation methods: 88.2g of toluene diisocyanate was dissolved in N, N-dimethylformamide as an organic solvent to form an isocyanate solution. 52.0g of aniline and 59.8g of p-toluidine were dissolved in N, N-dimethylformamide as an organic solvent to form an aromatic amine solution. The aromatic amine solution is added to the isocyanate solution, mixed and stirred well for reaction. And filtering and collecting the polyurea thickening agent, drying and grinding the polyurea thickening agent into powder. The polyurea thickening agent powder is mixed with 710g of PAO base oil, fully stirred and heated to 140-160 ℃ to form the lubricating grease. The temperature of the grease is reduced to 100 ℃ and 120 ℃, 5g of di-tert-butyl-p-cresol, 5g of alkyl phenyl-alpha-naphthylamine, 10g of zinc dialkyl dithiophosphate, 40g of dialkyl dithiocarbamate, 20g of barium dinonyl naphthalene sulfonate and 10g of polymethacrylate are added and stirred uniformly. And continuously cooling to normal temperature, homogenizing, degassing and filtering to obtain the finished product of the lubricating grease.
Example 5
The embodiment provides a lubricating grease composition for an electric automobile hub bearing, which comprises the following preparation methods: 41.2g of toluene diisocyanate and 64.9g of 4, 4' -diisocyanate diphenylmethane were dissolved in an organic solvent, N-dimethylformamide, to form an isocyanate solution. 48.3g of aniline and 55.6g of p-toluidine were dissolved in N, N-dimethylformamide as an organic solvent to form an aromatic amine solution. The aromatic amine solution is added to the isocyanate solution, mixed and stirred well for reaction. And filtering and collecting the polyurea thickening agent, drying and grinding the polyurea thickening agent into powder. The polyurea thickening agent powder is mixed with 700g of PAO base oil, fully stirred and heated to 140-160 ℃ to form the lubricating grease. The temperature of the lubricating grease is reduced to 100 ℃ and 120 ℃, 5g of di-tert-butyl-p-cresol, 5g of alkyl phenyl-alpha-naphthylamine, 25g of zinc dialkyl dithiophosphate, 25g of dialkyl dithiocarbamate, 20g of barium dinonyl naphthalene sulfonate and 10g of polymethacrylate are added and stirred uniformly. And continuously cooling to normal temperature, homogenizing, degassing and filtering to obtain the finished lubricating grease.
The parts by weight of the components of the grease compositions of examples 1-5 are shown in table 1.
Table 1 grease compositions of examples 1-5
Figure BDA0003136234180000081
Figure BDA0003136234180000091
Comparative example 1
The present comparative example provides a grease composition having the composition shown in Table 2, which was prepared as follows: 73.6g of toluene diisocyanate was dissolved in N, N-dimethylformamide as an organic solvent to form an isocyanate solution. 89.0g of cyclohexylamine was dissolved in an organic solvent, N-dimethylformamide to form an amine solution. The amine solution was added to the isocyanate solution, mixed and reacted with thorough stirring. And filtering and collecting the polyurea thickening agent, drying and grinding the polyurea thickening agent into powder. The polyurea thickening agent powder is mixed with 750g of PAO base oil, fully stirred and heated to 140 ℃ and 160 ℃ to form the lubricating grease. The temperature of the lubricating grease is reduced to 100 ℃ and 120 ℃, 5g of di-tert-butyl-p-cresol, 5g of alkyl phenyl-alpha-naphthylamine, 25g of zinc dialkyl dithiophosphate, 25g of dialkyl dithiocarbamate, 20g of barium dinonyl naphthalene sulfonate and 10g of polymethacrylate are added and stirred uniformly. And continuously cooling to normal temperature, homogenizing, degassing and filtering to obtain the finished product of the lubricating grease.
Comparative example 2
The present comparative example provides a grease composition having the composition shown in Table 2, which was prepared as follows: 27.3g of toluene diisocyanate and 43.3g of 4, 4' -diisocyanate diphenylmethane were dissolved in an organic solvent of N, N-dimethylformamide to form an isocyanate solution. 89.4g of N-octylamine was dissolved in an organic solvent, N-dimethylformamide, to form an amine solution. The amine solution was added to the isocyanate solution, mixed and the reaction stirred well. And filtering and collecting the polyurea thickening agent, drying and grinding the polyurea thickening agent into powder. And mixing the polyurea thickening agent powder with 750g of PAO base oil, fully stirring and heating to 140-160 ℃ to form lubricating grease. The temperature of the grease is reduced to 100 ℃ and 120 ℃, 5g of di-tert-butyl-p-cresol, 5g of alkyl phenyl-alpha-naphthylamine, 25g of zinc dialkyl dithiophosphate, 25g of dialkyl dithiocarbamate, 20g of barium dinonyl naphthalene sulfonate and 10g of polymethacrylate are added and stirred uniformly. And continuously cooling to normal temperature, homogenizing, degassing and filtering to obtain the finished product of the lubricating grease.
Comparative example 3
The present comparative example provides a grease composition having the composition shown in Table 2, which was prepared as follows: 39.2g of toluene diisocyanate and 61.8g of 4, 4' -diisocyanate diphenylmethane were dissolved in an organic solvent, N-dimethylformamide to form an isocyanate solution. 46.0g of aniline and 53.0g of p-toluidine were dissolved in N, N-dimethylformamide as an organic solvent to form an amine solution. The amine solution was added to the isocyanate solution, mixed and reacted with thorough stirring. And filtering and collecting the polyurea thickening agent, drying and grinding the polyurea thickening agent into powder. The polyurea thickening agent powder is mixed with 730g of mineral base oil, fully stirred and heated to 140 ℃ and 160 ℃ to form the lubricating grease. The temperature of the lubricating grease is reduced to 100 ℃ and 120 ℃, 5g of di-tert-butyl-p-cresol, 5g of alkyl phenyl-alpha-naphthylamine, 20g of zinc dialkyl dithiophosphate, 30g of dialkyl dithiocarbamate, 20g of barium dinonyl naphthalene sulfonate and 10g of polymethacrylate are added and stirred uniformly. And continuously cooling to normal temperature, homogenizing, degassing and filtering to obtain the finished product of the lubricating grease. The parts by weight of the components of the grease compositions of comparative examples 1-3 are shown in table 2.
TABLE 2 grease compositions of comparative examples 1 to 3
Figure BDA0003136234180000101
Figure BDA0003136234180000111
Test example 1
The grease compositions of examples 1-5 and comparative examples 1-3 were tested for their performance according to the following test methods, and the results are shown in Table 3.
The high-temperature resistance and oxidation resistance of the lubricating grease are measured by adopting a standard SH/T0428 method, and the test conditions are as follows: rotation speed 10000rpm, temperature 177 ℃. And judging the high-temperature-resistant and oxidation-resistant service life performance of the lubricating grease according to a high-temperature and high-speed service life bench test result.
The cold starting torque performance of the grease samples was determined using the method of standard SH/T0338, and the cold torque of the grease at-40 deg.C, including the starting torque and running torque, was determined. The test reflects the influence of the lubricating grease on the starting torque and the operating torque of the hub bearing of the electric automobile under the condition of low temperature.
The water-resistant antirust performance of the lubricating grease is measured by adopting a standard GB/T5018 method, and the analysis conditions are as follows: standing at 52 deg.C under relative humidity of 100% for 48 hr. The test reflects the ability of grease to prevent the hub bearing of an electric automobile from rusting under the action of temperature, moisture and air.
The extreme pressure antiwear performance of the lubricating grease is measured by adopting a standard SH/T0204 method. This test reflects the ability of the grease to withstand a load.
The method of standard GB/T269 is adopted to measure the anti-shearing performance of the lubricating grease, and the extension work of the lubricating grease is measured 105Difference between post-secondary cone penetration and working cone penetration (60 times). This test reflects the ability of the grease to maintain proper consistency against loss after repeated shearing.
The adhesion performance of the lubricating grease is measured by adopting a standard SH/T0109 method, water is sprayed to a bearing filled with the lubricating grease at a certain temperature (79 ℃) and flow rate (5mL/s), and the weight loss of the lubricating grease in the bearing is measured to evaluate the water spraying resistance of the lubricating grease. This test shows the adhesion of reactive greases.
Table 3 results of performance test of grease compositions in examples and comparative examples
Figure BDA0003136234180000112
Figure BDA0003136234180000121
As can be seen from the performance data in Table 3, the aromatic polyurea greases according to the present invention (examples 1 to 5) have more excellent performance than the alicyclic grease (comparative example 1) and the aliphatic grease (comparative example 2) in terms of the high-temperature life performance, the shear resistance, the adhesion performance, and the like of the greases compared to comparative examples 1 to 2 according to the present invention. Compared with comparative example 3, the lubricating grease provided by the invention has more excellent performance in the aspects of low-temperature starting torque and low-temperature running torque. The lubricating grease composition produced by the raw materials and the preparation method has excellent high-temperature-resistant oxidation resistance, low-temperature starting torque performance, water-resistant anti-rust performance, extreme pressure wear resistance and shear leakage resistance, and better meets the lubricating requirements of the hub bearing of the electric automobile.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (15)

1. The automobile hub bearing lubricating grease composition for the electric automobile is characterized by comprising base oil, a thickening agent and an additive, wherein the additive is one or more of an antioxidant, an extreme pressure anti-wear agent, an antirust agent and a tackifier; the base oil is PAO base oil, the thickening agent is an aromatic polyurea thickening agent, and the mass ratio of the base oil to the thickening agent is 70-75: 16 to 21; preparing the aromatic polyurea lubricating grease by adopting a prefabricated thickening agent method; the pre-preparation thickening agent method comprises the steps of respectively dissolving diisocyanate and aromatic amine in an organic solvent N, N-dimethylformamide, and stirring to obtain an isocyanate solution and an aromatic amine solution; mixing and reacting the isocyanate solution and the aromatic amine solution; then filtering, drying and grinding are carried out to obtain the aromatic polyurea thickening agent; the aromatic amine is aniline and p-toluidine.
2. The automobile hub bearing lubricating grease composition for electric vehicles according to claim 1, wherein the polyurea thickening agent is prepared from a mixture of polyurea and polyurea in a molar ratio of 0.5-8: 1 and diisocyanate to obtain the aromatic amine; the diisocyanate is toluene diisocyanate and/or 4, 4' -diisocyanate diphenylmethane.
3. The automobile hub bearing grease composition for electric vehicles according to claim 1, wherein the PAO base oil has a viscosity of 80 to 150mm at 40 ℃2The pour point is less than or equal to minus 40 ℃, and the viscosity index is more than or equal to 120.
4. The automobile hub bearing grease composition for electric vehicles according to claim 1, wherein the additive consists of an antioxidant, an extreme pressure anti-wear agent, an antirust agent and a tackifier.
5. The automobile hub bearing grease composition for electric vehicles according to claim 1, wherein the mass ratio of the antioxidant, the extreme pressure anti-wear agent, the antirust agent and the tackifier is 0.9-1.0: 4.5-5.0: 1.7-2.3: 0.9 to 1.0.
6. The automobile hub bearing grease composition for electric vehicles according to claim 4, wherein the antioxidant is a mixture of di-tert-butyl-p-cresol and alkylphenyl-alpha-naphthylamine; the mass ratio of the di-tert-butyl-p-cresol to the alkyl phenyl-alpha-naphthylamine is 0.1-10: 1; the mass of the antioxidant is 0.9-1.0% of the total mass of the composition.
7. The automobile hub bearing grease composition for electric vehicles according to claim 6, wherein the mass ratio of the di-tert-butyl-p-cresol to the alkylphenyl-alpha-naphthylamine is 1: 1.
8. the automobile hub bearing grease composition for electric vehicles according to claim 4, wherein the extreme pressure antiwear agent is one of zinc dialkyl dithiophosphate, dialkyl dithiocarbamate or a mixture thereof.
9. The automobile hub bearing grease composition for electric vehicles according to claim 8, characterized in that the weight of the extreme pressure antiwear agent is 4.5-5.0% of the total weight of the composition.
10. The automobile hub bearing grease composition for electric vehicles according to any one of claims 4 to 9, wherein the rust inhibitor is barium dinonylnaphthalene sulfonate.
11. The automobile hub bearing grease composition for electric vehicles according to claim 10, wherein the mass of the rust inhibitor is 1.7-2.3% of the total mass of the composition.
12. The automobile hub bearing grease composition for electric vehicles according to any one of claims 4 to 9, wherein the tackifier is polymethacrylate.
13. The automobile hub bearing grease composition for electric vehicles according to claim 12, characterized in that the mass of the tackifier is 0.9 to 1.0% of the total mass of the composition.
14. The automobile hub bearing grease composition for electric vehicles according to any one of claims 1 to 9, characterized in that the grease composition comprises the following components in parts by weight:
70-75 parts of PAO base oil;
16-21 parts of aromatic polyurea thickening agent;
0.9-1.0 part of antioxidant;
4.5-5.0 parts of an extreme pressure antiwear agent;
1.7-2.3 parts of an antirust agent;
0.9-1.0 part of tackifier.
15. The preparation method of the automobile hub bearing grease composition for electric vehicles according to any one of claims 1 to 14, which is characterized by comprising the following steps: mixing the polyurea thickening agent with PAO base oil, and then mixing with an additive; preparing the aromatic polyurea lubricating grease by adopting a prefabricated thickening agent method; the pre-preparation thickening agent method comprises the steps of respectively dissolving diisocyanate and aromatic amine in an organic solvent N, N-dimethylformamide, and stirring to obtain an isocyanate solution and an aromatic amine solution; mixing and reacting the isocyanate solution and the aromatic amine solution; then filtering, drying and grinding are carried out to obtain the aromatic polyurea thickening agent; mixing the aromatic polyurea thickening agent and the PAO base oil, and heating to 140-160 ℃ to form a lubricating grease precursor; cooling the lubricating grease precursor to 100-120 ℃, and mixing with the additive; and then continuously cooling, homogenizing, degassing and filtering to obtain the automobile hub bearing lubricating grease composition for the electric automobile.
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CN111073746A (en) * 2020-01-02 2020-04-28 中国石油化工股份有限公司 Polyurea-based hub bearing lubricating grease composition and preparation method and application thereof
CN112522005A (en) * 2019-09-17 2021-03-19 中国石油化工股份有限公司 Lubricating grease composition for electric automobile driving motor and preparation method thereof
CN112521997A (en) * 2019-09-17 2021-03-19 中国石油化工股份有限公司 Lubricating grease composition for metallurgical sintering machine and preparation method thereof

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