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CN117701324A - Pitting-resistant vehicle gear oil and preparation method thereof - Google Patents

Pitting-resistant vehicle gear oil and preparation method thereof Download PDF

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Publication number
CN117701324A
CN117701324A CN202311703214.0A CN202311703214A CN117701324A CN 117701324 A CN117701324 A CN 117701324A CN 202311703214 A CN202311703214 A CN 202311703214A CN 117701324 A CN117701324 A CN 117701324A
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China
Prior art keywords
pitting
vehicle gear
agent
gear oil
oil
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Inventor
黄红涛
徐文博
张兆钧
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Zheng Ji Suo Zhengzhou Transmission Technology Co ltd
Shanghai Advanced Research Institute of CAS
Zhengzhou Research Institute of Mechanical Engineering Co Ltd
Original Assignee
Zheng Ji Suo Zhengzhou Transmission Technology Co ltd
Shanghai Advanced Research Institute of CAS
Zhengzhou Research Institute of Mechanical Engineering Co Ltd
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Priority to CN202311703214.0A priority Critical patent/CN117701324A/en
Publication of CN117701324A publication Critical patent/CN117701324A/en
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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
    • 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
    • C10M169/04Mixtures of base-materials and additives
    • C10M169/048Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04Elements
    • C10M2201/041Carbon; Graphite; Carbon black
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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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    • 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
    • C10M2207/28Esters
    • C10M2207/283Esters of polyhydroxy compounds
    • C10M2207/2835Esters of polyhydroxy compounds used as base material
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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • 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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    • 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
    • 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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    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/02Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds
    • C10M2219/022Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds of hydrocarbons, e.g. olefines
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    • 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
    • C10M2223/041Triaryl phosphates
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • 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
    • C10M2223/043Ammonium or amine salts thereof
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    • 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
    • C10M2223/047Thioderivatives not containing metallic elements
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    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/04Detergent property or dispersant property
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    • 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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    • 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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    • 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
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    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/18Anti-foaming property
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    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/04Oil-bath; Gear-boxes; Automatic transmissions; Traction drives

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The invention discloses pitting corrosion resistant vehicle gear oil and a preparation method thereof, and belongs to the field of lubricating oil. The method comprises the following steps of: 88.0 to 95.0 percent of mixed base oil; extreme pressure agent 1.8-6.0%; 0.5 to 2.5 percent of antiwear agent; 0 to 0.15 percent of solid nano material; 1.5 to 3.5 percent of detergent dispersant; 0.1 to 0.2 percent of metal deactivator; 0.2 to 0.5 percent of antioxidant; 0.01 to 0.02 percent of anti-foaming agent. The preparation method comprises the following steps: under the protection of nitrogen, the solid nano material, the metal deactivator, the antiwear agent and the detergent dispersant are formed into a homogeneous dispersion system under the high temperature and high pressure condition, and then the homogeneous dispersion system is mixed with the extreme pressure agent and the antioxidant in proportion, cooled and filtered to obtain the pitting corrosion-resistant vehicle gear oil complexing agent. The vehicle gear oil can effectively improve the fatigue resistance of the electric drive vehicle gearbox.

Description

Pitting-resistant vehicle gear oil and preparation method thereof
Technical Field
The invention belongs to the technical field of lubricating oil, and particularly relates to anti-pitting vehicle gear oil and a preparation method thereof.
Background
The gear transmission refers to a device for transmitting motion and power by a gear pair, and is the most widely used mechanical transmission mode in various modern equipment. The contact stress generated by the alternating load of the tooth surface exceeds the limit stress of the surface or subsurface material during the gear transmission, and fatigue cracks can appear at corresponding positions. The fatigue crack is continuously expanded and extended, and finally the small block metal of the tooth surface is fallen off to form a pit, so that contact fatigue stripping is generated. Pitting, i.e., pitting or micropitting, of the tooth surface is a major feature of gear contact fatigue damage. The contact fatigue with a lower degree can cause the vibration enhancement and the noise enhancement of the gear during the work; when fatigue peeling is serious, the tooth can lose stability during meshing, an impact effect is generated, and broken teeth are easy to fail. More than 50% of the gear failure patterns are statistically associated with tooth breakage or pitting caused by contact fatigue.
The contact fatigue of gears is related to the materials of the gears, the manufacturing process, the tooth surface roughness, the working load, the lubrication condition and the lubricant performance. With the popularization of electrically driven vehicles, the wide use of power motors on vehicle power systems enables a large number of vehicle gearboxes to adopt single-gear or low-gear design, which leads to remarkable improvement of gear surface contact stress, great improvement of gearbox power density and more times of alternating load born by gears under the same mileage. Therefore, for an electric drive transmission with few gears, the probability of contact fatigue of gears is remarkably improved, and the reduction of gear transmission quality caused by contact fatigue is more likely to occur.
In the technical field of lubrication, contact fatigue resistance mainly prevents early pits from being generated, and prevents pitting or micro pitting. Industrial gear oils and complexing agents having a contact fatigue resistance function have been developed and developed in a large amount, and an invention has been made for an anti-micropitting industrial gear oil such as CN102766504A, CN102041140A, CN102031185 a. However, the requirements of the vehicle gear oil on the performance of impact load resistance, scratch resistance and the like are obviously higher than those of industrial gear oil, so that the industrial gear technical scheme of micro pitting corrosion resistance cannot be applied to the vehicle gear oil.
The traditional vehicle gear oil is mainly applied to a gear box and an axle of a vehicle, and because the tooth surface contact stress and alternating frequency of a multi-gear box are relatively low, the traditional vehicle gear oil mainly focuses on improving the extreme pressure wear resistance, heat resistance, oxidation resistance, environmental adaptability and other capabilities of the oil, and has no requirement on the micro pitting corrosion resistance of the oil. Although lubricating oil compositions having an anti-micro pitting function exist in the prior art, the lubricating oil compositions are mainly directed to dual clutch multi-speed transmissions of fuel vehicles. Compared with the traditional multi-gear gearbox, the gear number of the electric drive vehicle gearbox is obviously reduced, and the tooth surface contact stress and the alternating load frequency are obviously improved, so that the lubricating oil is difficult to meet the anti-fatigue requirement of the low-gear gearbox of the electric drive system of the new energy automobile.
In view of this, the present application is specifically proposed.
Disclosure of Invention
The invention aims to provide anti-pitting vehicle gear oil which is mainly applied to an electric drive vehicle few-gear transmission, can effectively solve the technical problem of fatigue resistance of the electric drive system few-gear transmission, realizes the balance of extreme pressure wear resistance and pitting resistance of oil products, and has excellent corrosion resistance.
The invention is realized by the following technical scheme:
in a first aspect, the present invention provides a pitting resistant vehicle gear oil comprising, in weight percent:
88.0 to 95.0 percent of mixed base oil;
extreme pressure agent 1.8-6.0%;
0.5 to 2.5 percent of antiwear agent;
0 to 0.15 percent of solid nano material; 1.5 to 3.5 percent of detergent dispersant;
0.1 to 0.2 percent of metal deactivator;
0.2 to 0.5 percent of antioxidant;
0.01 to 0.02 percent of anti-foaming agent.
Further, in a preferred embodiment of the present invention, the mixed base oil is 90.0 to 95.0% by weight; the extreme pressure agent is 2.3-5.0%; the antiwear agent is 1.0-2.0%; the detergent dispersant is 1.8-3.2%; 0.01 to 0.1 percent of solid nano material.
Further, in a preferred embodiment of the present invention, the antiwear agent includes at least one of a phosphate amine salt, a phosphite amine salt, a nitrogen-containing heterocyclic phosphite amine salt, tricresyl phosphate and a thiophosphate amine salt.
Further, in a preferred embodiment of the present invention, the extreme pressure agent includes at least one of sulfurized olefins, dibenzyldisulfide, sulfurized fatty oils, polyalkylbenzylsulfur compounds;
further, in a preferred embodiment of the present invention, the average particle size of the solid nanomaterial is less than 2000nm, including: at least one of nano diamond, nano metal, nano graphite, nano plastic and nano ceramic;
further, in a preferred embodiment of the present invention, the detergent dispersant comprises at least one of polyisobutylene succinimide and boronated polyisobutylene succinimide.
Further, in a preferred embodiment of the present invention, the metal deactivator includes at least one of benzotriazole derivatives, thiadiazole derivatives and imidazoline derivatives.
Further, in a preferred embodiment of the present invention, the mixed base oil includes at least one of a high viscosity index hydrofinished group III base oil, a polyolefin synthetic oil, and an ester synthetic oil.
Further, in a preferred embodiment of the present invention, the anti-foaming agent includes at least one of a silicone polymer and an organic polyether ester compound.
In a second aspect, the present application also provides a method for preparing anti-pitting vehicle gear oil, comprising:
stirring the solid nano material, the metal deactivator, the antiwear agent and the detergent dispersant for 2 hours under the protection of nitrogen at the pressure of 2.0-5.0 bar and the temperature of 250-350 ℃, cooling and filtering to form a homogeneous dispersion system, and obtaining the first complexing agent.
Mixing the first complexing agent, the extreme pressure agent and the antioxidant in proportion, stirring for 0.5-2 hours at 60-70 ℃ and 200-350 rpm, cooling, and filtering to obtain the pitting-resistant vehicle gear oil complexing agent;
mixing the mixed base oil, the anti-foaming agent and the anti-pitting vehicle gear oil complexing agent in proportion, and stirring for 1-3 hours at the temperature of 75-85 ℃ and the speed of 1000-1500 rpm to obtain the anti-pitting vehicle gear oil;
further, in a preferred embodiment of the present invention, the cooling step includes stirring and cooling at 200 to 350 rpm.
Compared with the prior art, the invention has at least the following technical effects:
the solid nano material, the metal deactivator, the antiwear agent and the detergent dispersant are stirred and mixed under high temperature and high pressure conditions, and the solid nano additive is combined with other additives through chemical reaction, so that a homogeneous system is formed. Overcomes the adverse phenomena of sedimentation, layering and the like of the solid nano material in the long-term storage process.
The vehicle gear oil has excellent extreme pressure wear resistance, durability, rust resistance and corrosion resistance; more importantly, the vehicle gear oil shows excellent pitting corrosion resistance in an actual bench test and a laboratory simulation test, can simultaneously meet the lubrication requirements of gears and bearings in a few-gear transmission of an electric drive vehicle, and can effectively improve the fatigue resistance of the gearbox of the electric drive vehicle. Of course, the vehicle gear oil can meet the lubrication requirements of gears and bearings in a vehicle multi-gear gearbox driven by fuel oil, and has wide application prospects.
Specifically, the solid nano material is added into the lubricating oil additive on the basis of reasonably selecting the composition and the proportion of the lubricating oil additive, and the pitting corrosion resistance effect of the lubricating oil additive is enhanced through the solid nano material. The mechanism of action is that nano solid material plays a supporting role on the gear surface, thereby improving the thickness of lubricating oil film and reducing the contact stress of the gear, and simultaneously converting the sliding friction part into rolling friction, thereby reducing the possibility of generating cracks on the gear surface, even if the cracks are generated, the pressure of oil wedges in the cracks is reduced due to the increased thickness of oil films of nano particles, thereby avoiding the expansion of the cracks, and in addition, nano metal particles can enter the cracks to realize crack repair, thereby reducing the occurrence probability of micro-pitting and pitting.
Drawings
FIG. 1 is a graph of the wear scar morphology after the simulated test of pitting resistance provided by compositions 1-5 of the examples of the present invention.
FIG. 2 shows an electrically driven gearbox for testing the fatigue resistance of oil in an experimental example of the invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the following examples, which are to be construed as merely illustrative and not limitative of the scope of the invention, but are not intended to limit the scope of the invention to the specific conditions set forth in the examples, either as conventional or manufacturer-suggested, nor are reagents or apparatus employed to identify manufacturers as conventional products available for commercial purchase.
The technical scheme of the embodiment is as follows:
the inventors found in practice that: the existing vehicle gear oil has higher extreme pressure wear resistance, heat resistance, oxidation resistance and environmental suitability, but has weaker micro pitting corrosion resistance. The vehicle gear oil can be applied to a double-clutch multi-gear gearbox of a fuel automobile, but is difficult to apply to an electrically driven vehicle gearbox with obviously improved tooth surface contact stress and alternating load frequency. For electrically driven new energy automobiles, the stability of the gears of the gearbox is directly related to the overall performance and life of the automobile.
In this regard, the present embodiment provides a pitting corrosion resistant vehicle gear oil comprising, in weight percent:
(A) 88.0 to 95.0 percent of mixed base oil;
(B) Extreme pressure agent 1.8-6.0%;
(C) 0.5 to 2.5 percent of antiwear agent;
(D) 0 to 0.15 percent of solid nano material;
(E) 1.5 to 3.5 percent of detergent dispersant;
(F) 0.1 to 0.2 percent of metal deactivator;
(G) 0.2 to 0.5 percent of antioxidant;
(H) 0.01 to 0.02 percent of anti-foaming agent.
Wherein, the components in the pitting corrosion resistant vehicle gear oil can be specifically:
the mixed base oil (a) includes at least one of a high viscosity index hydrofined group III base oil, a polyolefin synthetic oil, and an ester synthetic oil. That is, the mixed base oil comprises at least one high viscosity index hydrofinished group III base oil, or a polyolefin synthetic oil, or an ester synthetic oil, or any combination thereof. The mixed base oil is suitably present in the gear oil composition in an amount of 88.0wt% to 95.0wt%, preferably in an amount of 90.0wt% to 93.0wt%, for example 91.0wt%, 92.0wt% or 93.0wt%.
The extreme pressure agent (B) comprises a sulphurised olefin, which may comprise at least one high pressure sulphurised olefin isobutylene or a conventional sulphurised olefin isobutylene, or any combination of olefins. Wherein the traditional sulphurised alkene isobutene is traditional sulphurised alkene produced by two steps of sulphurisation and chlorination of isobutene; the high-pressure sulfurized olefin isobutylene is one-step high-pressure synthesized sulfur alkene. The extreme pressure agent is suitably contained in the gear oil composition in an amount of 1.8 to 6.0wt%; preferably, the content is 2.3wt% to 5.0wt%, for example, 2.5wt%, 3.0wt%, 3.5wt%, 4.0wt% or 4.5wt%.
The antiwear agent (C) includes at least one of a phosphate amine salt, a phosphite amine salt, a nitrogen-containing heterocyclic phosphite amine salt, tricresyl phosphate and a thiophosphate amine salt. In particular, the antiwear agent comprises at least one amine phosphate salt, or a phosphite salt, or a nitrogen-containing heterocyclic phosphite salt, or tricresyl phosphate, or a phosphorothioate salt, or any combination of the above. The suitable content of the antiwear agent in the gear oil composition is 0.5wt% to 2.0wt%; preferably, the content is 1.0 to 2.0wt%, for example, 1.4wt%, 1.6wt% or 1.8wt%.
The solid nanomaterial (D) comprises at least one of nanodiamond, nano metal, nano graphite, nano plastic, and nano ceramic. Specifically, the nano diamond is prepared by a detonation method; the nano metal comprises nano metal powder prepared from copper, iron, titanium, nickel, silver, aluminum, alloys or oxides thereof and the like; the nano plastic comprises nano particles prepared from plastics such as nano polyethylene, nano PET polyester, nano nylon 6 and the like; the nano ceramic comprises silicate ceramic, oxide ceramic, nitride ceramic, carbide ceramic, metal ceramic and the like; the proper content of the solid nano material in the gear oil composition is 0 to 0.15 weight percent; preferably, the content is 0.01wt% to 0.12wt%; more preferably, the content is 0.01wt% to 0.1wt%.
The detergent dispersant (E) comprises at least one of polyisobutylene succinimide and boronated polyisobutylene succinimide. Specifically, the detergent dispersant comprises at least one polyisobutylene succinimide, or a boronated polyisobutylene succinimide, or any combination of the above. The suitable content of the detergent dispersant in the gear oil composition is 1.5wt% -3.5 wt%; preferably, the content is 1.8wt% to 3.2wt%; more preferably, the content is 2.0wt% to 3.0wt%.
The metal deactivator (F) includes at least one of a benzotriazole derivative, a thiadiazole derivative and an imidazoline derivative. Specifically, the metal deactivator comprises at least one benzotriazole derivative, or a thiadiazole derivative, or an imidazoline derivative, or any combination of the above. Suitable levels of metal deactivator in the gear oil composition are from 0.1wt% to 0.2wt%, for example, may be 0.12wt%, 0.15wt%, or 0.18wt%.
The antioxidant (G) comprises at least one of 2, 6-di-tert-butyl-p-cresol, N-phenyl-a-naphthylamine, dioctyl diphenylamine and dialkyl dithiocarbamate. Specifically, the antioxidant comprises at least one of 2, 6-di-tert-butyl-p-cresol, or N-phenyl-a-naphthylamine, or dioctyl diphenylamine, or dialkyl dithiocarbamate, or any combination of the above. The antioxidant is suitably present in the gear oil composition in an amount of from 0.2wt% to 0.5wt%; preferably, the content is 0.3wt% to 0.4wt%.
The antifoaming agent (H) includes at least one of a silicone polymer and an organic polyether ester compound. In particular, at least one silicone polymer, or an organic polyether ester compound, or any combination of the above components. The suitable content of the anti-foaming agent in the gear oil composition is 0.01wt% to 0.02wt%; preferably, the content is 0.013wt% to 0.017wt%.
The embodiment also provides a preparation method of the pitting corrosion resistant vehicle gear oil, which comprises the following steps:
and S1, stirring the solid nano material, the metal deactivator, the antiwear agent and the detergent dispersant for 2 hours under the protection of nitrogen at the pressure of 2.0-5.0 bar and the temperature of 250-350 ℃, cooling and filtering to form a homogeneous dispersion system, and thus obtaining the first complexing agent.
S2, mixing the first complexing agent, the extreme pressure agent and the antioxidant in proportion, stirring for 0.5-2 hours at the temperature of 60-70 ℃ and the rpm of 200-350 rpm, cooling and filtering to obtain the pitting corrosion-resistant vehicle gear oil complexing agent.
S3, mixing the mixed base oil, the anti-foaming agent and the anti-pitting vehicle gear oil complexing agent in proportion, and stirring for 1-3 hours at 75-85 ℃ and 1000-1500 rpm to obtain the anti-pitting vehicle gear oil;
further, in a preferred embodiment of the present invention, the cooling step includes stirring and cooling at 200 to 350 rpm.
Wherein the viscosity, anti-foaming property and low temperature brookfield viscosity of the mixed base oil satisfy the following table 1:
TABLE 1 Performance index requirements of Mixed base oils
Further, in order to screen the base oil component and each additive component, the present invention tested oil performance in the laboratory by using a kinematic viscosity method (GB/T265), a copper flake corrosion test (GB/T5096), an anti-rust performance test of inhibitor-added mineral oil in the presence of water (GB/T11143), a four ball mill plaque diameter method (1200 RPM, 40Kg, 75 ℃ C., 60 min) (SH/T0189), a lubricant carrying capacity method (GB/T3142), an inductively coupled plasma emission spectrometry (GB/T17476) of additive elements, wear metals and contaminants in used lubricating oils and certain element assays in base oils, a lubricating oil insolubles assay (GB/T8926) in use, a standard test method for measuring iron wear debris monitoring in service fluids using a particle quantizer (ASTM/D8184), and the like.
In order to screen additive components, the invention mainly uses a high-frequency reciprocating friction tester to simulate and evaluate the pitting resistance of oil products in a laboratory. The specific test method comprises the following steps: under the condition of lubrication of an oil product to be tested, a friction pair adopts a ball plate contact mode to carry out tribology test, wherein a steel plate is fixed, a steel ball carries out high-frequency reciprocating motion, the load on the steel ball is loaded step by step in a gradient increasing mode, each stage of load test is the same in duration, the appearance of a grinding mark after a specific load test is observed and photographed, the pitting area percentage of the surface of the grinding mark is calculated, and the test is terminated if severe abrasion occurs in the test process. And the pitting resistance of the oil products is judged by comparing the pitting area percentages of the surface of the grinding mark of different oil products under the same load condition.
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
Examples 1 to 2
The components and contents of the pitting corrosion resistant vehicle gear oil composition are shown in table 2:
TABLE 2 Components and contents of vehicle Gear oil composition
The preparation method of the composition 1 comprises the following steps: the components in Table 2 were directly stirred at 75 to 80℃to form a mixture, which was filtered and cooled to obtain composition 1.
The preparation method of the composition 2 comprises the following steps:
and step A, stirring the solid nano material, the metal deactivator, the antiwear agent and the detergent dispersant in the table 2 for 2 hours under the protection of nitrogen at the pressure of 2.0-5.0 bar and the temperature of 250-350 ℃, cooling and filtering to form a homogeneous dispersion system, and thus obtaining the first complexing agent.
And step B, mixing the first complexing agent with the extreme pressure agent and the antioxidant shown in the table 2 in proportion, stirring for 0.5-2 hours at the temperature of 60-70 ℃ and the rpm of 200-350 rpm, cooling and filtering to obtain the pitting corrosion-resistant vehicle gear oil complexing agent.
And C, mixing the mixed base oil, the anti-foaming agent and the anti-pitting vehicle gear oil complexing agent in proportion, and stirring for 1-3 hours at the temperature of 75-85 ℃ and the speed of 1000-1500 rpm to obtain the anti-pitting vehicle gear oil composition 2.
Compositions 1 and 2 were stored under the same conditions, composition 1 became cloudy and precipitated after 7 days, while composition 2 was clear after 6 months, indicating that the preparation of composition 2 significantly improved the stability of the oil.
Examples 3 to 6
The anti-pitting vehicle gear oils provided in examples 3-6 were substantially identical in composition 2 in terms of their components and preparation methods, except that the antiwear agent was selected (1.0 wt% in each case) in order to examine the effect of the difference in antiwear agent on the performance of the gear oil. The components and performance test results are shown in fig. 1 and table 3:
TABLE 3 simulation test results of pitting resistance of compositions 1 to 5
Examples Antiwear agent Observing load/N Percentage of pitting/%
Example 2 Tricresyl phosphate 600 1.33
Example 3 Phosphoric acid ester amine salt 600 0.42
Example 4 Amine salts of phosphorothioates 600 0
Example 5 Dialkyl dithiophosphate 600 20.04
Example 6 Zinc dialkyldithiophosphate 600 8.46
As can be seen from Table 3, the phosphorothioate amine salt and the tricresyl phosphate in the antiwear agent have good pitting resistance; among them, the pitting resistance with the phosphorothioate amine salt is the best. Whereas the dialkyl dithiophosphate and zinc dialkyl dithiophosphate have poor pitting resistance.
Examples 7 to 9
Examples 7-9 provide pitting resistant vehicle gear oils that are substantially identical to composition 2, except that: the selection and content of each component are shown in table 4:
TABLE 4 Components and contents of examples 4-6
Wherein, the kinematic viscosity (cSt) in the mixed base oil refers to the kinematic viscosity at 100 ℃.
The lubricating oils provided in examples 7 to 9 were subjected to a simulation evaluation of pitting resistance by a high-frequency reciprocating friction tester, and the results are shown in Table 5.
TABLE 5 simulation test results of the viscosity temperature and pitting resistance of the lubricating oils of examples 7 to 9
As can be seen from Table 5, the increased viscosity of the gear oil is beneficial to improving the pitting resistance of the gear oil, and the high-pressure vulcanized olefin can improve the pitting resistance of the oil product compared with the normal-pressure vulcanized olefin.
Examples 10 to 14
Examples 10-14 provide pitting resistant vehicle gear oils that are substantially identical to composition 2, except that: the selection and content of each component are shown in table 6:
TABLE 6 Components and contents of examples 10-14
The gear oils provided in examples 10-14 were subjected to a simulated evaluation of pitting resistance and the results are shown in Table 7.
TABLE 7 results of Performance test of examples 10-14
As can be seen from Table 7, the addition of nanodiamond can improve the abrasion and pitting resistance of the oil (examples 10 and 11); too high a pressure sulfurized isobutylene content would result in increased pitting corrosion (examples 10 and 12); an excessively high phosphorothioate amine salt content, although better in pitting resistance, leads to deterioration in corrosion and rust resistance (examples 10 and 13); the balance of corrosion resistance, rust resistance, abrasion resistance and pitting resistance can be realized by reasonably collocating the phosphate amine salt and the thiophosphate amine salt.
Experimental example 1
To comprehensively evaluate the application effects of the additive components and the lubricating oil composition, the present invention conducted fatigue resistance tests on lubricating oil example 7, example 14 and comparative oil samples, respectively, on electrically driven gearbox benches.
Wherein, the contrast oil is: conventional multi-speed transmission GL-5 80W-90 vehicle gear oil (produced as a lubricating oil for too-wide) is commercially available.
The test gearbox is an electrically driven single-gear gearbox (figure 2), and an accelerated fatigue test is carried out for 80 hours under a high torque condition so as to realize the simulation test of the full life cycle of the gearbox. And collecting oil after the bench test is finished, and analyzing performances such as abrasive dust, elements and the like in the collected oil, so that the actual service performance of the oil is comprehensively judged. Table 5 shows the results of bench oil tests, wherein the PQ index reflects the content of ferromagnetic particles with the diameter of more than 10 microns in the oil, and the iron element in the element content test mainly reflects the content of element iron with the diameter of less than 10 microns. Because the contact fatigue pitting of the gear is a pit formed by the peeling of the metal of the tooth surface, the PQ index in the oil product can reflect the pitting degree of the tooth surface, and meanwhile, the elemental iron with small particle size (less than 10 microns) is mainly generated by the abrasion of the tooth surface, so that the content of the elemental iron can reflect the abrasion resistance of the oil product.
The test results are shown in table 8:
TABLE 8 bench oil test results
As can be seen from Table 8, after 80 hours of fatigue resistance bench test, the oil of example 14 has smaller contents of ferromagnetic particles and iron elements than those of example 7 and comparative oil, indicating that the oil has better wear resistance and fatigue resistance.
Finally, it should be noted that: the foregoing description is only of the preferred embodiments of the invention and is not intended to limit the scope of the invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1.一种抗点蚀车辆齿轮油,其特征在于,按照重量百分比计,其包括:1. An anti-pitting corrosion vehicle gear oil, characterized in that, in terms of weight percentage, it includes: 混合基础油88.0~95.0%;Mixed base oil 88.0~95.0%; 极压剂1.8~6.0%;Extreme pressure agent 1.8~6.0%; 抗磨剂0.5~2.5%;Anti-wear agent 0.5~2.5%; 固体纳米材料0~0.15%;Solid nanomaterials 0~0.15%; 清净分散剂1.5~3.5%;Detergent dispersant 1.5~3.5%; 金属减活剂0.1~0.2%;Metal deactivator 0.1~0.2%; 抗氧剂0.2~0.5%;Antioxidant 0.2~0.5%; 抗泡剂0.01~0.02%。Anti-foaming agent 0.01~0.02%. 2.根据权利要求1所述的抗点蚀车辆齿轮油,其特征在于,按照重量百分比计,所述混合基础油为90.0~95.0%;所述极压剂为2.3~5.0%;所述抗磨剂为1.0~2.0%;所述清净分散剂为1.8~3.2%;所述固体纳米材料0.01~0.1%。2. The anti-pitting vehicle gear oil according to claim 1, characterized in that, in terms of weight percentage, the mixed base oil is 90.0-95.0%; the extreme pressure agent is 2.3-5.0%; and the anti-pitting agent is 2.3-5.0%. The grinding agent is 1.0-2.0%; the detergent dispersant is 1.8-3.2%; the solid nanomaterial is 0.01-0.1%. 3.根据权利要求1或2所述的抗点蚀车辆齿轮油,其特征在于,所述抗磨剂包括磷酸酯胺盐、亚磷酸酯胺盐、含氮杂环亚磷酸酯胺盐、磷酸三甲酚酯和硫代磷酸酯胺盐中的至少一种。3. The anti-pitting vehicle gear oil according to claim 1 or 2, characterized in that the anti-wear agent includes phosphate amine salt, phosphite amine salt, nitrogen-containing heterocyclic phosphite amine salt, phosphoric acid At least one of tricresol ester and phosphorothioate amine salt. 4.根据权利要求1或2所述的抗点蚀车辆齿轮油,其特征在于,所述极压剂包括硫化烯烃、二苄基二硫醚、硫化脂肪油和多烷基苄硫化合物中的至少一种。4. The anti-pitting vehicle gear oil according to claim 1 or 2, characterized in that the extreme pressure agent includes sulfurized olefins, dibenzyl disulfide, sulfurized fatty oil and polyalkyl benzyl sulfide compounds. At least one. 5.根据权利要求1或2所述的抗点蚀车辆齿轮油,其特征在于,所述固体纳米材料的平均粒径小于2000nm,包括纳米金刚石、纳米金属、纳米石墨、纳米塑料和纳米陶瓷中的至少一种。5. The anti-pitting vehicle gear oil according to claim 1 or 2, characterized in that the average particle size of the solid nanomaterial is less than 2000nm, including nanodiamond, nanometal, nanographite, nanoplastic and nanoceramics. of at least one. 6.根据权利要求1或2所述的抗点蚀车辆齿轮油,其特征在于,所述清净分散剂包括聚异丁烯丁二酰亚胺和硼化聚异丁烯丁二酰亚胺中的至少一种。6. The anti-pitting vehicle gear oil according to claim 1 or 2, characterized in that the detergent dispersant includes at least one of polyisobutylene succinimide and boronized polyisobutylene succinimide. . 7.根据权利要求1或2所述的抗点蚀车辆齿轮油,其特征在于,所述金属减活剂包括苯三唑衍生物、噻二唑衍生物和咪唑啉衍生物中的至少一种。7. The anti-pitting vehicle gear oil according to claim 1 or 2, characterized in that the metal deactivator includes at least one of benzene triazole derivatives, thiadiazole derivatives and imidazoline derivatives . 8.根据权利要求1或2所述的抗点蚀车辆齿轮油,其特征在于,所述混合基础油包括高粘度指数加氢精制III类基础油、聚烯烃合成油和酯类合成油中的至少一种。8. The anti-pitting vehicle gear oil according to claim 1 or 2, characterized in that the mixed base oil includes high viscosity index hydrorefined Group III base oil, polyolefin synthetic oil and ester synthetic oil. At least one. 9.根据权利要求1或2所述的抗点蚀车辆齿轮油,其特征在于,所述抗泡剂包括有机硅聚合物和有机聚醚酯化合物中的至少一种。9. The anti-pitting vehicle gear oil according to claim 1 or 2, wherein the anti-foaming agent includes at least one of a silicone polymer and an organic polyetherester compound. 10.一种根据权利要求1-9任一项所述的抗点蚀车辆齿轮油的制备方法,其特征在于,其包括:10. A method for preparing anti-pitting vehicle gear oil according to any one of claims 1-9, characterized in that it includes: 在氮气保护条件下,于2.0~5.0bar压力和250~350℃温度条件下将所述固体纳米材料、金属减活剂、抗磨剂和清净分散剂搅拌2小时,冷却、过滤后形成均相分散体系,得到第一复合剂;Under nitrogen protection conditions, stir the solid nanomaterials, metal deactivators, anti-wear agents and clean dispersants for 2 hours at a pressure of 2.0 to 5.0 bar and a temperature of 250 to 350°C, then cool and filter to form a homogeneous phase. Disperse the system to obtain the first compound agent; 再将第一复合剂与所述极压剂和抗氧剂按比例混合,于60~70℃、200~350rpm下搅拌0.5~2h,冷却、过滤得到抗点蚀车辆齿轮油复合剂;Then mix the first compound agent with the extreme pressure agent and antioxidant in proportion, stir at 60-70°C and 200-350 rpm for 0.5-2 hours, cool and filter to obtain an anti-pitting vehicle gear oil compound agent; 将所述混合基础油、抗泡剂与抗点蚀车辆齿轮油复合剂按比例混合,于75~85℃、1000~1500rpm下搅拌1~3h,得到抗点蚀车辆齿轮油。Mix the mixed base oil, anti-foaming agent and anti-pitting vehicle gear oil compound in proportion, and stir at 75-85°C and 1000-1500 rpm for 1 to 3 hours to obtain anti-pitting vehicle gear oil.
CN202311703214.0A 2023-12-12 2023-12-12 Pitting-resistant vehicle gear oil and preparation method thereof Pending CN117701324A (en)

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