CN111394158A - Extreme pressure antiwear transmission engine oil and preparation method thereof - Google Patents
Extreme pressure antiwear transmission engine oil and preparation method thereof Download PDFInfo
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- CN111394158A CN111394158A CN202010213595.4A CN202010213595A CN111394158A CN 111394158 A CN111394158 A CN 111394158A CN 202010213595 A CN202010213595 A CN 202010213595A CN 111394158 A CN111394158 A CN 111394158A
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- 230000005540 biological transmission Effects 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
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- 239000003921 oil Substances 0.000 claims abstract description 33
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- 238000003825 pressing Methods 0.000 claims abstract description 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 90
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C—CHEMISTRY; METALLURGY
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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- C10M2201/08—Inorganic acids or salts thereof
- C10M2201/081—Inorganic acids or salts thereof containing halogen
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/102—Silicates
- C10M2201/103—Clays; Mica; Zeolites
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- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/16—Paraffin waxes; Petrolatum, e.g. slack wax
- C10M2205/163—Paraffin waxes; Petrolatum, e.g. slack wax used as base material
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/30—Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids
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- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/08—Macromolecular 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
- C10M2209/084—Acrylate; Methacrylate
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/086—Imides
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- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/02—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2217/024—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an amido or imido group
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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/02—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds
- C10M2219/022—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds of hydrocarbons, e.g. olefines
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- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/047—Thioderivatives not containing metallic elements
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- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/049—Phosphite
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/02—Unspecified siloxanes; Silicones
Abstract
The invention discloses extreme pressure antiwear transmission engine oil and a preparation method thereof. The preparation method of the extreme pressure anti-wear gearbox oil comprises the following steps: step one, preparing materials; step two: mixing the other raw materials except the special defoaming agent for the lubricating oil in the step one, then adding the special defoaming agent for the lubricating oil, stirring and mixing, and naturally cooling to room temperature to obtain a mixture; step three: and D, performing filter pressing on the mixture obtained in the step two to obtain the extreme pressure anti-wear gearbox engine oil. The extreme pressure anti-wear transmission engine oil disclosed by the invention has excellent anti-corrosion performance, thermal oxidation stability, sealing adaptability, anti-wear durability and extreme pressure anti-wear performance, can simultaneously meet the requirements of lubrication of manual transmissions of high-grade cars, and lubrication of manual transmissions of vehicles, trucks and buses, and can achieve the purposes of prolonging the service cycle of the transmission engine oil, reducing the maintenance frequency of equipment, saving energy, reducing consumption and reducing cost.
Description
Technical Field
The invention relates to the technical field of gear oil, in particular to extreme pressure anti-wear gearbox oil and a preparation method thereof.
Background
An automatic transmission is a transmission device that can automatically perform an automatic shift operation in accordance with a vehicle speed and an engine speed, which occurs in contrast to a manual transmission. At present, four types of automatic transmissions for automobiles are common, namely a hydraulic automatic transmission, a mechanical stepless automatic transmission, an electric control mechanical automatic transmission and a double-clutch automatic transmission. The automatic transmission oil is called automatic transmission oil for short, and is oil liquid specially used for an automatic transmission. Early automatic transmissions did not have dedicated oil, but instead were replaced with engine oil. Because of the wide variation in operating conditions and specifications, engine oils are rapidly being eliminated as an automatic transmission fluid. The special oil liquid for the automatic transmission used at present is not only transmission oil of a hydraulic torque converter, but also lubricating oil of a planetary gear structure and hydraulic oil of a gear shifting device. The automatic transmission oil in the prior art has the defects of short service life, poor lubricating effect, easiness in foaming, no oxidation resistance, poor antirust performance and the like.
Application number 201610832394.6 relates to a powershift transmission oil composition, consisting of the following components in percentage by weight: 0.1-0.2% of alkyl diphenylamine; 0.2-0.3% of liquid phenol antioxidant; 9.0-10.0% of multifunctional composite additive; 0.5-1.0% of pour point depressant; 0.1-0.2% of a friction modifier; 0-0.04% of an antifoaming agent; the kinematic viscosity is 10.0-11.5 mm2The balance of base oil/s. The lubricating oil has extremely high viscosity index, excellent high oxidation resistance and long service life of the friction plate, and has the effect of prolonging the service life of the friction plate by more than one time compared with the common power gear shifting transmission oil.
Application number 201711270380.0 discloses an automatic transmission oil, which is composed of the following raw materials by mass percent: 0.1-0.9% of an antiwear agent, 0.3-1.4% of an antioxidant, 0.5-1.5% of molybdenum dialkyl dithiocarbamate, 0.2-0.6% of a defoaming agent, and the balance of base oil. The automatic transmission oil disclosed by the invention is reasonable in proportion, has a good lubricating effect in a low-temperature state, can improve the friction performance of an oil product, has good anti-shaking performance, and can improve the discomfort problem experienced by a driver.
Application number 201810674718.7 discloses an automatic transmission oil comprising the following components in parts by weight: 75-90 parts of base oil; 2-5 parts of viscosity index improver; 2-4 parts of a detergent dispersant; 0.5-1.5 parts of antioxidant; 0.1-0.2 part of metal deactivator; 1-2 parts of an antiwear agent; 1-1.5 parts of dialkyl dithiocarbamate; 0.1-0.5 part of defoaming agent. The lubricating grease has excellent lubricating property, oxidation stability and low-temperature fluidity, has good abrasion resistance and clean dispersing property, does not foam, and prolongs the service life.
Disclosure of Invention
The automatic transmission oil is mainly used for automatic transmission systems of cars and light trucks, along with the rapid development of the manufacturing industry of automatic transmissions, the requirements on the automatic transmission oil in the market are increasingly improved, and the extreme pressure anti-wear property, the low-temperature flow property and the oxidation stability are all important indexes for inspecting the automatic transmission oil, but most of the automatic transmission oil in the current market has the defects of short service life, easiness in foaming, poor lubricating effect, no oxidation resistance, poor cleaning and dispersing property and general friction property, and cannot meet the requirements of the market.
In order to solve the problems, the invention provides a preparation method of extreme pressure anti-wear gearbox oil, which comprises the following steps:
the method comprises the following steps: preparing materials according to the following mixture ratio: 3-7 parts of a composite material of nano montmorillonite and a polymer, 0.3-0.8 part of a composite antirust antioxidant, 2.0-3.8 parts of vulcanized isobutylene, 0.1-0.5 part of a special defoaming agent for lubricating oil, 0.5-1.0 part of a bis-alkoxy monothiophosphate ester triazine derivative, 1-5 parts of polyisobutylene bis-succinimide, 0.1-0.2 part of thiophosphate amine salt, 0.5-2 parts of an antiwear agent, 1-2 parts of a fluorine-containing additive and 70-130 parts of base oil;
step two: mixing the raw materials except the special defoaming agent for the lubricating oil in the step one, stirring for 30-60 minutes at 50-80 ℃, then adding the special defoaming agent for the lubricating oil, stirring for 10-30 minutes at 50-80 ℃, and naturally cooling to room temperature to obtain a mixture;
step three: and D, performing filter pressing on the mixture obtained in the step two under the condition of 0.3-0.5 MPa to obtain the extreme pressure anti-wear gearbox engine oil.
In some technical schemes of the invention, the composite material of the nano montmorillonite and the polymer uses the nano montmorillonite as a carrier, and the nano montmorillonite is organically modified by cetyl trimethyl ammonium bromide to obtain organically modified nano montmorillonite; then polymerizing and grafting monomers of octadecyl methacrylate and acrylamide into the montmorillonite layer to synthesize the nano-montmorillonite composite viscosity reducer.
The preparation process of the composite material of the nano montmorillonite and the polymer comprises the following steps:
pretreatment of reactants and initiators
(1) Purification of reactant octadecyl methacrylate: washing octadecyl methacrylate with a sodium hydroxide aqueous solution with the mass fraction of 5-10% until the octadecyl methacrylate is colorless, then repeatedly washing with distilled water until the washing liquid is neutral, and performing vacuum drying to obtain purified octadecyl methacrylate, and storing in a brown reagent bottle for storage;
(2) and (2) purifying the initiator azobisisobutyronitrile, namely adding 50-200 m of L volume percent ethanol aqueous solution with volume fraction of 95% into a three-neck flask provided with a reflux condenser tube, heating until the ethanol is nearly boiled, quickly adding 5-20 g of azobisisobutyronitrile, stirring until the azobisisobutyronitrile is completely dissolved, carrying out suction filtration while hot, cooling to obtain white crystals, carrying out vacuum drying, and storing the purified azobisisobutyronitrile in a brown reagent bottle for cold storage and standby.
Organic modification of II nano montmorillonite
(1) Adding 0.1-5 g of nano montmorillonite into 10-100 m L distilled water, stirring for 2-4 hours, and standing until complete swelling to obtain a montmorillonite aqueous solution;
(2) adding 5-30 m L distilled water into 5-10 g of intercalation agent hexadecyl trimethyl ammonium bromide, and stirring until the mixture is completely dissolved to obtain an intercalation agent aqueous solution;
(3) placing the montmorillonite aqueous solution in a water bath at 50-70 ℃ for heat preservation for 2-3 hours, then adding an intercalator aqueous solution, performing heat preservation reaction at 50-70 ℃ for 4-8 hours, cooling to room temperature, performing centrifugal separation, and collecting bottom precipitate; and (4) drying the bottom precipitate in vacuum to obtain the organic modified montmorillonite.
Preparation of composite material of III nano montmorillonite and polymer
Adding organic modified montmorillonite into absolute ethyl alcohol according to a solid-liquid ratio of 1 (50-100) (g/m L), carrying out ultrasonic treatment for 30-60 minutes to obtain a dispersion liquid, sequentially adding acrylamide and octadecyl methacrylate into the dispersion liquid, wherein the organic modified montmorillonite accounts for 5-7% of the total mass of the acrylamide and the octadecyl methacrylate, the molar ratio of the acrylamide to the octadecyl methacrylate is (1-3) to 1, introducing nitrogen, carrying out heat preservation at 60-80 ℃ for 0.5-1 hour, then adding an initiator azobisisobutyronitrile, wherein the initiator azobisisobutyronitrile accounts for 0.3-0.75% of the total mass of the acrylamide and the octadecyl methacrylate, carrying out reaction at 60-80 ℃ for 4-6 hours, carrying out centrifugal separation on the reaction liquid, collecting a bottom solid, and carrying out vacuum drying on the bottom solid to obtain the composite material of the nano montmorillonite and the polymer.
In some technical schemes of the invention, the composite material of the nano montmorillonite and the polymer uses the nano montmorillonite as a carrier, and the nano montmorillonite is organically modified by sodium dodecyl benzene sulfonate to obtain organically modified nano montmorillonite; then polymerizing and grafting monomers of octadecyl methacrylate, N-hydroxymethyl acrylamide and maleic anhydride into the montmorillonite layer to synthesize the nano-montmorillonite composite viscosity reducer.
The preparation process of the composite material of the nano montmorillonite and the polymer comprises the following steps:
pretreatment of reactants and initiators
(1) Purification of reactant octadecyl methacrylate: washing octadecyl methacrylate with a sodium hydroxide aqueous solution with the mass fraction of 5-10% until the octadecyl methacrylate is colorless, then repeatedly washing with distilled water until the washing liquid is neutral, and performing vacuum drying to obtain purified octadecyl methacrylate, and storing in a brown reagent bottle for storage;
(2) and (2) purifying the initiator azobisisobutyronitrile, namely adding 50-200 m of L volume percent ethanol aqueous solution with volume fraction of 95% into a three-neck flask provided with a reflux condenser tube, heating until the ethanol is nearly boiled, quickly adding 5-20 g of azobisisobutyronitrile, stirring until the azobisisobutyronitrile is completely dissolved, carrying out suction filtration while hot, cooling to obtain white crystals, carrying out vacuum drying, and storing the purified azobisisobutyronitrile in a brown reagent bottle for cold storage and standby.
Organic modification of II nano montmorillonite
(1) Adding 0.1-5 g of nano montmorillonite into 10-100 m L distilled water, stirring for 2-4 hours, standing until the nano montmorillonite is completely swelled, and adjusting the pH to be neutral by using 0.1-1 mol/L hydrochloric acid to obtain a montmorillonite aqueous solution;
(2) adding 5-30 m L distilled water into 5-10 g of anionic surfactant sodium dodecyl benzene sulfonate, and stirring until the distilled water is completely dissolved to obtain an anionic surfactant aqueous solution;
(3) placing the montmorillonite aqueous solution in a water bath at 50-70 ℃ for heat preservation for 2-3 hours, then adding an anionic surfactant aqueous solution, performing heat preservation reaction at 50-70 ℃ for 4-8 hours, cooling to room temperature, performing centrifugal separation, and collecting bottom precipitate; and (4) drying the bottom precipitate in vacuum to obtain the organic modified montmorillonite.
Preparation of composite material of III nano montmorillonite and polymer
Adding organic modified montmorillonite into absolute ethyl alcohol according to a solid-liquid ratio of 1 (50-100) (g/m L), carrying out ultrasonic treatment for 30-60 minutes to obtain a dispersion liquid, sequentially adding octadecyl methacrylate, N-hydroxymethyl acrylamide and maleic anhydride into the dispersion liquid, introducing nitrogen into the dispersion liquid, keeping the temperature of the mixture at 60-80 ℃ for 0.5-1 hour, adding azodiisobutyronitrile serving as an initiator, wherein the molar ratio of the N-hydroxymethyl acrylamide to the octadecyl methacrylate to the maleic anhydride is (1-3): 1 (0.2-0.7), reacting at 60-80 ℃ for 4-6 hours, carrying out centrifugal separation on the reaction liquid, collecting bottom solids, and carrying out vacuum drying on the bottom solids to obtain the composite material of the nano montmorillonite and the polymer.
The preparation principle of the composite material viscosity reducer of the nano montmorillonite and the polymer is as follows: firstly, adding water to swell dry montmorillonite, and then organically modifying the montmorillonite by using an auxiliary agent at a certain temperature to ensure that auxiliary agent molecules enter montmorillonite layers through the ion exchange effect, thereby enlarging the interlayer spacing of the montmorillonite. The organic ions generally contain long-chain alkyl groups, and the long-chain alkyl groups can be filled in the montmorillonite layers, so that the original hydrophilicity of the inner and outer montmorillonite layers is changed into hydrophobicity, the montmorillonite layers can be fused with organic substances, the specific surface area of the montmorillonite layers is increased due to the enlarged interlayer spacing, and the organic substances can be introduced into the interlayers, so that the nano-montmorillonite and polymer composite viscosity reduction material is synthesized.
The viscosity reducer of the composite material of the nano montmorillonite and the polymer obtained by the two technical schemes has the following characteristics:
(1) the viscosity reducer of the nano montmorillonite composite material can be used as a nucleation point of paraffin wax crystallization due to the small size effect and the special nucleation effect of the nano material, so as to prevent the crystallization of the paraffin wax to form a larger wax block; meanwhile, strong polar groups are introduced between montmorillonite layers, hydrogen bonds can be formed through the action of colloid and asphaltene of the thick oil, the colloid asphalt is prevented from forming a three-dimensional network structure, the condensation point and viscosity of the thick oil are reduced through the combined action of the colloid and the asphaltene, and the low-temperature fluidity of the thick oil is improved.
(2) The second technical scheme is that a new monomer is introduced on the basis of using acrylamide and octadecyl methacrylate as polymerization monomers, so that the polymer molecular chain of the viscosity reducer molecule is lengthened, and the montmorillonite layer is filled with organic polymers as much as possible, thereby increasing the diversity of organic viscosity reducing components and polar groups, and improving the grafting rate and viscosity reducing effect.
(3) In natural montmorillonite layers, a large amount of inorganic metal ions exist, the cations can be replaced, when hexadecyl trimethyl ammonium bromide is used for modifying the montmorillonite layers, strong van der Waals force can be formed in the organic cation time, and the organic cation has certain hydrophobicity, so the organic cation can replace the inorganic metal cations among the montmorillonite layers to further generate organic montmorillonite, but anionic surfactants can be adsorbed among other layers. The second technical scheme is different from the method that cetyl trimethyl ammonium bromide is used for carrying out organic modification on montmorillonite, an anionic surfactant dodecyl benzene sulfonate is used for carrying out organic modification on the montmorillonite, negative ions in water can adsorb particles with negative charges among montmorillonite layers, meanwhile, C-H bonds in surfactant branched chains can form hydrogen bonds with molecules with stronger non-polarity among montmorillonite layers to be attached together, when a certain amount of negative ions are adsorbed among the montmorillonite layers, the density of the negative charges among the montmorillonite layers is increased, the repulsive force is increased, and therefore the interlayer spacing of the montmorillonite is increased.
Further, the fluorine-containing additive is a surface-modified nano lanthanum fluoride solid additive, and the preparation process comprises the steps of dissolving 8-12 g of lanthanum chloride solid in 300-600 m L distilled water, heating to 50-70 ℃, adding 30-50 m L mol concentration ammonia fluoride solution with the concentration of 1-5 mmol/L into the solution, reacting at 50-70 ℃ for 2-4 hours, adding 0.1-1 g of surface modifier into the reaction liquid after the reaction is completed, reacting at 50-70 ℃ for 1-2 hours, stopping heating and stirring, collecting the reaction liquid, naturally cooling the reaction liquid to room temperature, and carrying out vacuum freeze drying to finally obtain the surface-modified nano lanthanum fluoride solid additive.
The fluorine-containing additive is a surface-modified nano lanthanum fluoride liquid additive, and the preparation process comprises the steps of placing 15-30 g of oleic acid and 5-8 g of methanol into a three-neck flask with a reflux condenser, sequentially adding 0.1-0.3 g of toluenesulfonic acid as a catalyst and 2-5 m of L m of petroleum ether as a water-carrying agent, heating to 80-90 ℃, reacting at 80-90 ℃ under a heat preservation condition until no water is generated, so as to obtain a methyl oleate modifier, dissolving 8-12 g of lanthanum chloride solid in 300-600 m of L distilled water, heating to 50-70 ℃, adding an ammonia fluoride solution with a molar concentration of 1-5 mmol/L of 30-50 m of L into the solution, reacting at 50-70 ℃ for 2-4 hours, after the reaction is completed, adding 0.1-1 g of the surface modifier into a reaction liquid, reacting at 50-70 ℃ for 1-2 hours, so as to obtain a surface-modified lanthanum fluoride colloid, adding 0.1-1 g of the surface modifier into the reaction liquid, sequentially adding 0.539-10 g of the surface-modified lanthanum fluoride into the reaction liquid at 50-60 ℃, and drying the obtained colloid after the reaction is carried out under a heat preservation condition, so as a nano ammonium bromide liquid, so as a nano lanthanum-10 nanometer lanthanum-10 nanometer lanthanum-containing colloid, and drying, so as to obtain a nanometer lanthanum-10 nanometer.
In the above preparation scheme of the fluorine-containing additive, the surface modifier is one of KH560, oleic acid, cetyl trimethyl ammonium bromide, citric acid and stearic acid. The surface modifier is preferably KH 560.
The fluorine-containing additive used in the invention has excellent wear resistance by virtue of a special electronic structure of rare earth elements and a unique crystal structure of rare earth compounds, but solid particles have a large specific surface area due to extremely fine grains, so that a large surface energy is formed, in addition, attractive force exists among the particles, and the particles have a tendency of automatic aggregation3The powder additive has better dispersion stability and high-temperature stability.
Further, the base oil is one of Lanzhou petrochemical intermediate base oil MVIS600, Dalian petrochemical paraffin base oil HVI650, Daqing hydro-isodewaxing base oil HVIW H350 and poly alpha-olefin synthetic oil PAO-10.
The antiwear agent is an ionic liquid functionalized carbon quantum dot and is prepared by the steps of adding 3-5 g of ionic liquid into a reaction device, heating to 230-260 ℃ under the protection of nitrogen, adding 0.5-2 g of citric acid monohydrate under stirring, reacting for 4-10 hours at 230-260 ℃, naturally cooling to room temperature, adding 20-30 m of L distilled water, stirring for 2-3 hours to obtain a water dispersion, dialyzing the dispersion for 3-4 days by using a dialysis bag with the molecular weight cutoff of 1000-2000 Da, changing water every half day, removing water in the dialysate, and performing vacuum drying at 50-60 ℃ to obtain the ionic liquid functionalized carbon quantum dot.
In the preparation of the ionic liquid functionalized carbon quantum dot, the ionic liquid is 1-N-butyl-3-methylimidazolium tetrafluoroborate ionic liquid and/or N-butylpyridinium tetrafluoroborate ionic liquid. Preferably, the ionic liquid is a mixture of 1-N-butyl-3-methylimidazolium tetrafluoroborate ionic liquid and N-butylpyridinium tetrafluoroborate ionic liquid in a mass ratio of 1: 1.
In the prior art, traditional carbon nano-additive such as fullerene, carbon tube and graphene is usually used as an antiwear component, but because of surface inertia, the carbon nano-additive is usually required to be subjected to more complicated surface pretreatment before being used after being prepared, and the pretreatment not only consumes time but also greatly increases cost. In addition, fullerene is difficult to realize monodispersion in base liquid due to strong agglomeration capacity, and exists in a cluster form; the carbon tubes and graphene are not uniform in size; this makes the traditional nano carbon material still have a great promotion space for the embedding stability between the surface asperities of the friction interface. The invention forms a boundary lubricating film in the friction process by means of the synergistic lubricating effect between the carbon quantum dots and the ionic liquid, thereby greatly reducing the friction and the abrasion of a friction interface.
The second technical problem to be solved by the invention is to provide extreme pressure antiwear transmission engine oil.
The extreme pressure anti-wear gearbox oil is processed by using any one of the preparation methods of the extreme pressure anti-wear gearbox oil.
The extreme pressure anti-wear transmission engine oil disclosed by the invention has excellent anti-corrosion performance, thermal oxidation stability, sealing adaptability, anti-wear durability and extreme pressure anti-wear performance, can meet the lubricating requirement of a manual transmission of a high-grade car, and can simultaneously meet the lubricating requirement of a manual transmission of a vehicle drive axle, a truck and a bus, and can achieve the purposes of prolonging the service cycle of the transmission engine oil, reducing the maintenance frequency of equipment, saving energy, reducing consumption and reducing cost.
Detailed Description
The raw materials in the examples are as follows:
octadecyl methacrylate, CAS No.: 32360-05-7.
Azobisisobutyronitrile, CAS number: 78-67-1.
Nanometer montmorillonite, Autai mineral processing factory of Lingshou county, with 1250 mesh.
Cetyl trimethylammonium bromide, CAS number: 57-09-0.
Acrylamide, CAS No.: 79-06-1.
Sodium dodecylbenzenesulfonate, CAS No.: 25155-30-0.
N-methylolacrylamide, CAS No.: 924-42-5.
Maleic anhydride, CAS No.: 108-31-6.
Lanthanum chloride, CAS No.: 10099-58-8, 1000 mesh, Jinan Wanduoxin chemical Co., Ltd.
Oleic acid, CAS number: 112-80-1.
Toluene sulfonic acid, CAS No.: 104-15-4.
Tetrabutylammonium bromide, CAS No.: 1643-19-2.
Citric acid monohydrate, CAS No.: 77-92-9.
The basic criteria for the four base oils used in the examples are as follows:
examples 1 to 5
The preparation method of the extreme pressure anti-wear gearbox oil comprises the following steps:
preparing 4 parts by weight of a composite material of nano montmorillonite and a polymer, 0.3 part by weight of a composite antirust antioxidant (obtained by uniformly mixing an antirust agent (A L OX2188, the main component of sodium petroleum sulfonate, manufactured by Kunshan Tada chemical Co., Ltd.) and a phosphite type antioxidant (Qingdajie good new material science Co., Ltd.) and a phenol type antioxidant 1010 (manufactured by Toguan Confucius Giu de chemical Co., Ltd.) in a mass ratio of 3: 2: 2), 0.19 part by weight of sulfurized isobutylene (T321, manufactured by Runsheng chemical science Co., Ltd.), 0.5 part by weight of a special antifoaming agent for lubricating oil (product DF-anti-wear, manufactured by san Frangda Defeng antifoaming agent Co., Ltd., Sheng, the main component of polyether modified organosilicon), 0.5 part by weight of a bis-alkoxy monothiophosphate triazine derivative (refer to the research on tribology of bis-alkoxy monothiophosphate triazine derivative (which is described in 2005) and 0.5 part by weight of a bis-sulfo phosphate ester (CAS additive) (obtained by preparing 0.5 parts by using a commercially available chemical engineering additive (HVD.S. TM., S. TM., SOT 2, 2: 1000 parts by weight of a petrochemical industry Co., SOT 2, 2: 2, 2 parts by weight of a high molecular weight of a commercially available chemical additive (CAS additive, 3.3.3-3, 2, 3, 2, 3, 2;
step two: mixing the paraffin-based base oil HVI650, the composite material of the nano montmorillonite and the polymer, the composite antirust antioxidant, the sulfurized isobutylene, the bis-alkoxy monosulfur phosphate ester-based triazine derivative, the dispersing agent, the thiophosphate amine salt, the antiwear agent and the fluorine-containing additive in a stirrer, stirring for 40 minutes at 70 ℃, then adding the lubricating oil antifoaming agent, stirring for 20 minutes at 70 ℃, and naturally cooling to room temperature to obtain a mixture;
step three: and (4) filtering the mixture obtained in the step two under the pressure of 0.3MPa to obtain the extreme pressure anti-wear gearbox oil.
The preparation process of the composite material of the nano montmorillonite and the polymer comprises the following steps:
pretreatment of reactants and initiators
(1) Purification of reactant octadecyl methacrylate: washing octadecyl methacrylate with a sodium hydroxide aqueous solution with the mass fraction of 5% until the octadecyl methacrylate is colorless, then repeatedly washing with distilled water until the washing liquid is neutral, and performing vacuum drying at 50 ℃ for 24 hours to obtain purified octadecyl methacrylate, and storing in a brown reagent bottle for cooling for later use;
(2) and (3) purifying the initiator azobisisobutyronitrile, namely adding 100m of ethanol aqueous solution with the volume fraction of L and the volume fraction of 95% into a three-neck flask with a reflux condenser, heating until the ethanol is nearly boiled, quickly adding 10g of azobisisobutyronitrile, stirring at 100 revolutions per minute until the azobisisobutyronitrile is completely dissolved, carrying out suction filtration while the solution is hot, cooling to obtain white crystals, carrying out vacuum drying at 50 ℃ for 12 hours, and storing the purified azobisisobutyronitrile in a brown reagent bottle for storage and later use.
Organic modification of II nano montmorillonite
(1) Adding 1g of nano montmorillonite into 20m L of distilled water, stirring for 2 hours at 100 revolutions per minute, and standing for 24 hours until complete swelling to obtain montmorillonite aqueous solution;
(2) adding 10m L distilled water into 7g of intercalation agent hexadecyl trimethyl ammonium bromide, and stirring at 100 revolutions per minute until the intercalation agent is completely dissolved to obtain an intercalation agent aqueous solution;
(3) placing montmorillonite aqueous solution in water bath at 60 ℃ for heat preservation for 2 hours, then adding intercalation agent aqueous solution, simultaneously carrying out heat preservation reaction at 60 ℃ for 6 hours, cooling to room temperature, centrifuging for 30 minutes at 5000 revolutions per minute, and collecting bottom precipitate; and (3) drying the bottom precipitate at 50 ℃ for 6 hours in vacuum to obtain the organic modified montmorillonite.
Preparation of composite material of III nano montmorillonite and polymer
Adding organic modified montmorillonite into absolute ethyl alcohol according to a solid-liquid ratio of 1: 60(g/m L), carrying out ultrasonic treatment for 40 minutes under the conditions of ultrasonic power of 300W and ultrasonic frequency of 25kHz to obtain a dispersion liquid, sequentially adding acrylamide and octadecyl methacrylate into the dispersion liquid, wherein the organic modified montmorillonite accounts for 7 percent of the total mass of the acrylamide and the octadecyl methacrylate, the molar ratio of the acrylamide to the octadecyl methacrylate is 2: 1, introducing nitrogen, carrying out heat preservation for 0.5 hour at 60 ℃, then adding an initiator azobisisobutyronitrile, the initiator azobisisobutyronitrile accounts for 0.75 percent of the total mass of the acrylamide and the octadecyl methacrylate, carrying out reaction for 4 hours at 60 ℃, centrifuging the reaction liquid for 30 minutes at 5000 r/min, collecting bottom solids, and carrying out vacuum drying on the bottom solids for 12 hours at 50 ℃ to obtain the composite material of the nano montmorillonite and the polymer.
The antiwear agent is a carbon quantum dot functionalized by ionic liquid, and is prepared by adding 4g of ionic liquid (specifically 1-n-butyl-3-methylimidazolium tetrafluoroborate ionic liquid is used, and the ionic liquid is prepared according to the research on synthesis of 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid (Liuhongxia, chemical world, 11 th 2006) into a reaction device, wherein the reaction temperature is 80 ℃, the reaction time is 18 hours, the microwave power is 240W, the molar ratio of reactants is 1: 1: 1), heating to 260 ℃ at 5 ℃/min under the protection of nitrogen, adding 1g of citric acid monohydrate under the stirring condition of 100 revolutions per minute, reacting for 6 hours at 260 ℃, naturally cooling to room temperature, adding 25m L distilled water, stirring for 2 hours at 100 revolutions per minute to obtain an aqueous dispersion, dialyzing the dispersion for 3 days by using a dialysis bag with the molecular weight of 1000Da, changing water every half day, and finally removing water in the dialysate, and vacuum drying for 12 hours at 60 ℃ to obtain the carbon quantum dot functionalized by the ionic liquid.
The fluorine-containing additive is a surface-modified nano lanthanum fluoride solid additive, and the preparation process comprises the steps of dissolving 10g of lanthanum chloride solid in 500m L distilled water, heating to 60 ℃ at the speed of 2 ℃/min, dropwise adding 40m L molar concentration of 1 mmol/L ammonium fluoride solution into the solution at the speed of 0.3m L/min, reacting for 2 hours at the temperature of 60 ℃, adding 0.1g of surface modifier into the reaction solution after the reaction is completed, stopping heating and stirring after the reaction is carried out for 1 hour at the temperature of 60 ℃, collecting the reaction solution, naturally cooling the reaction solution to room temperature, and carrying out vacuum freeze drying to finally obtain the surface-modified nano lanthanum fluoride solid additive.
Examples 1 to 5 differ in that: the surface modifying agents used in the fluorine-containing additives of examples 1 to 5 were different. The surface modifiers used in examples 1 to 5 were oleic acid, stearic acid, cetyltrimethylammonium bromide, citric acid, and KH560, respectively.
The dispersion stabilizer of the fluorine-containing additive in the paraffin-based base oil HVI650 was tested: adding a fluorine-containing additive accounting for 1.6 percent of the weight of the paraffin base oil HVI650 into the paraffin base oil HVI650, carrying out ultrasonic treatment for 30 minutes, heating to 35 ℃, and stirring for 2 hours to prepare lubricating oil; adding the lubricating oil into a centrifuge tube, centrifuging for 10 minutes at four rotating speeds of 500 revolutions per minute, 1000 revolutions per minute, 2000 revolutions per minute and 3000 revolutions per minute by adopting a desktop centrifuge, and observing the precipitation condition of the lubricating oil in the centrifuge tube.
The specific test results are shown in table 1.
TABLE 1 Dispersion stability of fluorine-containing additives in paraffinic base oil HVI650
Example 6
The preparation method of the extreme pressure anti-wear transmission engine oil is the same as that in the embodiment 5, and the difference is that:
the preparation process of the composite material of the nano montmorillonite and the polymer comprises the following steps:
i, pretreatment of reactants and an initiator: the pretreatment process was the same as in examples 1 to 5.
Organic modification of II nano montmorillonite
(1) Adding 1g of montmorillonite into 40m L distilled water, stirring for 2 hours at 100 r/min, standing for 24 hours until complete swelling, and adjusting the pH to be neutral by using 0.1 mol/L hydrochloric acid to obtain a montmorillonite aqueous solution;
(2) adding 10m L distilled water into 7g of anionic surfactant sodium dodecyl benzene sulfonate, and stirring at 100 revolutions per minute until the mixture is completely dissolved to obtain an anionic surfactant aqueous solution;
(3) putting the montmorillonite aqueous solution into a water bath at 60 ℃ for heat preservation for 2 hours, then adding an anionic surfactant aqueous solution into the montmorillonite aqueous solution, simultaneously carrying out heat preservation reaction at 60 ℃ for 6 hours, cooling to room temperature, centrifuging for 30 minutes at 5000 revolutions per minute, and collecting bottom sediment; and (3) drying the bottom precipitate at 50 ℃ for 6 hours in vacuum to obtain the organic modified montmorillonite.
Preparation of composite material of III nano montmorillonite and polymer
Adding organic modified montmorillonite into absolute ethyl alcohol according to a solid-liquid ratio of 1: 60(g/m L), carrying out ultrasonic treatment for 40 minutes under the conditions of ultrasonic power of 300W and ultrasonic frequency of 25kHz to obtain a dispersion liquid, sequentially adding octadecyl methacrylate, N-hydroxymethyl acrylamide and maleic anhydride into the dispersion liquid, wherein the organic modified montmorillonite accounts for 7 percent of the total mass of octadecyl methacrylate, N-hydroxymethyl acrylamide and maleic anhydride, the molar ratio of N-hydroxymethyl acrylamide to octadecyl methacrylate to maleic anhydride is 2: 1: 0.5, introducing nitrogen and carrying out heat preservation for 0.5 hour at 80 ℃, then adding an initiator of azobisisobutyronitrile, the initiator of azobisisobutyronitrile accounts for 0.75 percent of the total mass of octadecyl methacrylate, N-hydroxymethyl acrylamide and maleic anhydride, carrying out reaction for 5 hours at 60 ℃, centrifuging the reaction liquid for 30 minutes at 5000 revolutions per minute to collect a bottom solid, and carrying out vacuum drying for 12 hours at 50 ℃ to obtain the composite material of nano montmorillonite and polymer.
Example 7
The preparation method of the extreme pressure antiwear transmission engine oil is the same as that of example 5.
The preparation process of the composite material of the nano montmorillonite and the polymer is the same as that of the example 6.
The fluorine-containing additive is a surface modified nano lanthanum fluoride liquid additive, and the preparation process comprises the steps of placing 20g of oleic acid and 5.5g of methanol into a three-mouth flask provided with a reflux condenser tube, sequentially adding 0.1g of toluenesulfonic acid as a catalyst and 2m L petroleum ether as a water-carrying agent, heating to 80 ℃ at a speed of 2 ℃/min, carrying out heat preservation reaction at 80 ℃ until no water is generated, stopping the reaction to obtain a methyl oleate modifier, dissolving 10g of lanthanum chloride solid into 500m L distilled water, heating to 60 ℃ at a speed of 2 ℃/min, dropwise adding 40m L mol concentration 1 mmol/L ammonia fluoride solution into the solution at a speed of 0.3m L/min, carrying out reaction at 60 ℃ for 2 hours, after the reaction is completed, adding 0.1g of KH560 into the reaction solution, carrying out reaction at 60 ℃ for 1 hour to obtain surface modified lanthanum fluoride, adding a surface modified lanthanum fluoride colloid into the methyl oleate modifier at 60 ℃, sequentially adding 0.09g of tetrabutyl ammonium bromide as a phase transfer catalyst and 5m of petroleum ether, carrying out heat preservation reaction at 60 ℃ for 1 hour, and drying the lanthanum fluoride liquid to obtain a surface modified lanthanum fluoride liquid, and carrying out heat preservation reaction at 50 hours, and drying at 60 ℃ to obtain a nano lanthanum fluoride liquid additive.
Examples 8 to 10
The formula and preparation method of the extreme pressure antiwear transmission engine oil are the same as those of example 7.
The differences are as follows: the base oils used in the formulation of the extreme pressure anti-wear transmission motor oil were different, and the base oil used in example 7 was the major petrochemical paraffin base oil HVI650, the base oil used in example 8 was the lanzhou petrochemical intermediate base oil MVIS600, the base oil used in example 9 was the major hydro-isodewaxing base oil HVIW H350, and the base oil used in example 10 was the poly a-olefin synthetic oil PAO-10.
Example 11
The method is basically the same as example 7, except that the antiwear agent is an ionic liquid functionalized carbon quantum dot, and is prepared by adding 4g of an ionic liquid (specifically, N-butylpyridintetrafluoroborate ionic liquid is used, and the ionic liquid is prepared according to research on synthesis of N-butylpyridintetrafluoroborate (Sun Seawa, chemical reagent, 6 months 2009) into a reaction device, wherein the molar ratio of pyridine to N-butyl bromide is 1: 1.2, the reaction temperature is 75 ℃, the reaction time is 12 hours, and the solvent is 20m L acetonitrile), heating to 260 ℃ at 5 ℃/min under the protection of nitrogen, adding 1g of citric acid monohydrate under the stirring condition of 100 revolutions per minute, reacting for 6 hours at 260 ℃, naturally cooling to room temperature, adding 25m L distilled water, stirring for 2 hours at 100 revolutions per minute to obtain an aqueous dispersion, dialyzing the dispersion for 3 days with a dialysis bag with the molecular weight cutoff of 1000Da, changing water every half day, and finally removing water in the dialysis solution, and vacuum drying at 60 ℃ for 12 hours to obtain the carbon quantum dot functionalized ionic liquid.
Example 12
The method is basically the same as example 7, except that the antiwear agent is an ionic liquid functionalized carbon quantum dot, and is prepared by adding 4g of ionic liquid into a reaction device, heating to 260 ℃ at 5 ℃/min under the protection of nitrogen, adding 1g of citric acid monohydrate under the stirring condition of 100 revolutions/min, reacting for 6 hours at 260 ℃, naturally cooling to room temperature, adding 25m L distilled water, stirring for 2 hours at 100 revolutions/min to obtain an aqueous dispersion, dialyzing the dispersion for 3 days by using a dialysis bag with the molecular weight cutoff of 1000Da, changing water every half day, finally removing water in the dialysate, and vacuum drying at 60 ℃ for 12 hours to obtain the ionic liquid functionalized carbon quantum dot.
The ionic liquid is a mixture of 1-N-butyl-3-methylimidazole tetrafluoroborate ionic liquid and N-butylpyridine tetrafluoroborate ionic liquid in a mass ratio of 1: 1.
The 1-n-butyl-3-methylimidazolium tetrafluoroborate ionic liquid is prepared by referring to the synthesis research of 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid (Liuhongxia, chemical world, 11 th 2006), the reaction temperature is 80 ℃, the reaction time is 18 hours, the microwave power is 240W, and the molar ratio of reactants is 1: 1: 1.
the N-butylpyridinium tetrafluoroborate ionic liquid is prepared by referring to the research on synthesis of ionic liquid N-butylpyridinium tetrafluoroborate (Sun sea, chemical reagent, 6 months 2009), wherein the molar ratio of pyridine to N-bromo-butane is 1: 1.2, the reaction temperature is 75 ℃, the reaction time is 12 hours, and the solvent is 20m L acetonitrile.
Test example 1
Four-ball friction and wear test experiments are carried out on the extreme pressure wear-resistant gearbox engine oil of the embodiment 5-11: the testing device of the four-ball testing machine is provided with 4 small balls, one steel ball at the upper part is connected with the main rotating shaft through a fixing device, and three steel balls at the lower part are tightly clamped in the oil cup. A steel ball on the upper part is respectively in point contact with three balls (called lower test balls for short) on the lower part, under a certain extrusion force, the main rotating shaft on the upper part rotates to drive the upper ball to perform sliding friction with the fixed lower test balls, and a grinding spot is left after the lower test steel ball is rubbed.
The steel ball for the test is a special steel ball with the diameter of 12.7mm for a four-ball machine, and is made of the following materials: GCr15 bearing steel, hardness: 60-63 HRC.
The characteristics of tribological properties mainly include coefficient of friction, Wear Scar Diameter (WSD), maximum non-seizing load (P)B). Wherein the maximum non-seizing load (P) is predominantB) The measurement of (1) is that under the experimental condition, the maximum load added by the steel ball without clamping is represented by the load intensity which can be born by the oil film. Under low load, the diameter of the wear scar of the steel ball is in direct proportion to the load, and the friction surface of the steel ball has a complete oil film in a low load range; when the load reaches PBAt this time, the wear scar diameter rises sharply. P of lubricating oilBThe larger the value, the stronger the bearing capacity of the oil film formed on the friction surface.
Maximum no-seize load (P)B) The test method (2): according to GB/T12583-1998, under a certain load, the rotating speed is 1350 revolutions per minute, the time is 10s, and the temperature is normal temperature. Measurement of PBDuring the test, after each test, the grinding marks of the three lower test balls need to be observed by using a microscope, whether the grinding marks are circular or not is observed, the diameter of the grinding marks is read, and the measurement requirements are met only by judging that the grinding marks of the steel balls are circular and do not exceed the maximum grinding mark diameter under the load, so that the load can be continuously increased for testing until the grinding marks of the steel balls do not meet the measurement requirements, and the loaded load is the final PBThe value is obtained.
The friction coefficient and the abrasion spot diameter are measured by the following method: referring to SH/T0762-2005 method, the rotation speed is 1200 r/min, the load is 392N, the temperature is normal temperature, the test time is60 min, the friction coefficient value of each second is obtained after the experiment, and the final friction coefficient is obtained by averaging the values; the wear scar diameters of 3 test balls were measured simultaneously, and the average value was taken as the final measured wear scar diameter in mm.
The specific test results are shown in table 2.
TABLE 2 four-ball wear test table
As can be seen from Table 2, the four ball sintering loads (PD) for the solvent refined oils (MVIS600 and HVIS650) are significantly higher than for the hydroisomerized dewaxed base oil (HVIWH350) and the synthetic base oil (PAO-10). This is because the solvent refined base oils contain natural sulfur-containing extreme pressure components, whereas the hydroisomerized dewaxed base oils are substantially free of natural sulfur-containing extreme pressure components, and synthetic oils do not contain natural sulfur-containing extreme pressure components. Furthermore, the four-ball speck values (D392N60min) for the solvent refined oils (MVIS600 and HVIS650) were significantly lower than for the hydroisomerized dewaxed base oil (HVIWH350) and the synthetic base oil (PAO-10) because the solvent refined base oils contained natural nitrogen-containing antiwear components.
Test example 2
The artificial aging test is carried out on the extreme pressure antiwear transmission engine oil of the embodiments 5 to 7 and 11 to 12: 100g of extreme pressure antiwear transmission engine oil test oil is added into a beaker, the beaker is placed in a constant temperature oven for 192 hours at the constant temperature of 150 ℃, and the viscosity change rate (%) and the phosphorus consumption rate (%) of the oil are measured.
Phosphorus consumption rate (before phosphorus test-after phosphorus test)/before phosphorus test × 100%.
The specific test results are shown in table 3.
TABLE 3 test table for artificial aging test
Test example 3
Copper sheet corrosion and anti-foaming tests were performed on the extreme pressure anti-wear transmission engine oils of examples 5 to 7 and examples 11 to 12.
The specific test results are shown in table 4.
TABLE 4 copper sheet Corrosion and anti-foaming test table
It should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art will be able to make the description as a whole, and the embodiments may be appropriately combined to form other embodiments as will be appreciated by those skilled in the art.
Claims (10)
1. The preparation method of the extreme pressure anti-wear gearbox oil is characterized by comprising the following steps:
the method comprises the following steps: preparing materials according to the following mixture ratio: 3-7 parts of a composite material of nano montmorillonite and a polymer, 0.3-0.8 part of a composite antirust antioxidant, 2.0-3.8 parts of vulcanized isobutylene, 0.1-0.5 part of a special defoaming agent for lubricating oil, 0.5-1.0 part of a bis-alkoxy monothiophosphate ester triazine derivative, 1-5 parts of polyisobutylene bis-succinimide, 0.1-0.2 part of thiophosphate amine salt, 0.5-2 parts of an antiwear agent, 1-2 parts of a fluorine-containing additive and 70-130 parts of base oil;
step two: mixing the raw materials except the special defoaming agent for the lubricating oil in the step one, stirring for 30-60 minutes at 50-80 ℃, then adding the special defoaming agent for the lubricating oil, stirring for 10-30 minutes at 50-80 ℃, and naturally cooling to room temperature to obtain a mixture;
step three: and D, performing filter pressing on the mixture obtained in the step two under the condition of 0.3-0.5 MPa to obtain the extreme pressure anti-wear gearbox engine oil.
2. The preparation method of the extreme pressure anti-wear gearbox oil as recited in claim 1, wherein the nano montmorillonite is used as a carrier in the composite material of the nano montmorillonite and the polymer, and the nano montmorillonite is organically modified by cetyl trimethyl ammonium bromide to obtain organically modified nano montmorillonite; then polymerizing and grafting monomers of octadecyl methacrylate and acrylamide into the montmorillonite layer to synthesize the nano-montmorillonite composite viscosity reducer.
3. The preparation method of the extreme pressure anti-wear transmission engine oil according to claim 1, characterized in that the nano montmorillonite and polymer composite material uses nano montmorillonite as a carrier, and the nano montmorillonite is organically modified by sodium dodecyl benzene sulfonate to obtain organically modified nano montmorillonite; then polymerizing and grafting monomers of octadecyl methacrylate, N-hydroxymethyl acrylamide and maleic anhydride into the montmorillonite layer to synthesize the nano-montmorillonite composite viscosity reducer.
4. The preparation method of the extreme pressure anti-wear gearbox oil as recited in claim 1, wherein the fluorine-containing additive is a surface-modified nano lanthanum fluoride solid additive, and the preparation method comprises the steps of dissolving 8-12 g of lanthanum chloride solid in 300-600 m L distilled water, heating to 50-70 ℃, adding 30-50 m L mol concentration ammonia fluoride solution with 1-5 mmol/L into the solution, reacting at 50-70 ℃ for 2-4 hours, adding 0.1-1 g of surface modifier into the reaction solution after the reaction is completed, stopping heating and stirring after the reaction is carried out at 50-70 ℃ for 1-2 hours, collecting the reaction solution, naturally cooling the reaction solution to room temperature, and carrying out vacuum freeze drying to obtain the surface-modified nano lanthanum fluoride solid additive.
5. The preparation method of the extreme pressure anti-wear transmission engine oil according to claim 1, wherein the fluorine-containing additive is a surface-modified nano lanthanum fluoride liquid additive, and the preparation method comprises the steps of placing 15-30 g of oleic acid and 5-8 g of methanol into a three-neck flask provided with a reflux condenser tube, sequentially adding 0.1-0.3 g of toluenesulfonic acid as a catalyst and 2-5 m of L petroleum ether as a water-carrying agent, heating to 80-90 ℃, reacting at 80-90 ℃ under a heat preservation condition until no water is generated, stopping the reaction to obtain a methyl oleate modifier, dissolving 8-12 g of lanthanum chloride solid in 300-600 m of L distilled water, heating to 50-70 ℃, adding an ammonia fluoride solution with a molar concentration of 1-5 mmol/L of 30-50 m of L into the solution, reacting at 50-70 ℃ for 2-4 hours, after the reaction is completed, adding 0.1-1 g of the surface modifier into a reaction liquid, reacting at 50-70 ℃ for 1-2 hours to obtain a surface-modified lanthanum fluoride colloid, transferring the lanthanum fluoride colloid into a surface-modified liquid after the reaction is completely reacted for 1-2 hours, and heating the lanthanum fluoride colloid to obtain a nano ammonium bromide liquid additive, and drying the lanthanum-10 nano ammonium bromide liquid after the lanthanum colloid is added into the reaction at 50-10 ℃ under a vacuum condition that the temperature of 50-4 hours, and the lanthanum-10 nanometer lanthanum-10 is sequentially heated, and the nano ammonium bromide liquid is.
6. The method of preparing an extreme pressure anti-wear transmission engine oil according to claim 4 or 5, wherein the surface modifier is one of KH560, oleic acid, cetyl trimethylammonium bromide, citric acid, and stearic acid.
7. The method of making an extreme pressure anti-wear transmission machine oil according to claim 6, wherein the surface modifier is KH 560.
8. The method of preparing the extreme pressure anti-wear transmission engine oil according to claim 6, wherein the base oil is one of Lanzhou petrochemical intermediate base oil MVIS600, Dalian petrochemical paraffinic base oil HVI650, Daqing hydroisomerization dewaxing base oil HVIW H350, and poly alpha-olefin synthetic oil PAO-10.
9. The preparation method of the extreme pressure anti-wear gearbox oil as claimed in claim 1, wherein the anti-wear agent is an ionic liquid functionalized carbon quantum dot, and the preparation method comprises the steps of adding 3-5 g of ionic liquid into a reaction device, heating to 230-260 ℃ under the protection of nitrogen, adding 0.5-2 g of citric acid monohydrate under the stirring condition, reacting for 4-10 hours at 230-260 ℃, naturally cooling to room temperature, adding 20-30 m L distilled water, stirring for 2-3 hours to obtain a water dispersion, dialyzing the dispersion for 3-4 days by using a dialysis bag with the molecular weight of cut-off being 1000-2000 Da, changing water once every half day, and finally removing water in the dialyzed solution, and performing vacuum drying at 50-60 ℃ to obtain the ionic liquid functionalized carbon quantum dot.
10. An extreme pressure anti-wear transmission machine oil, which is characterized by being processed by the preparation method of the extreme pressure anti-wear transmission machine oil according to any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112391221A (en) * | 2020-10-20 | 2021-02-23 | 凯盛石墨碳材料有限公司 | Anion-regulated carbon quantum dot and preparation and application methods thereof |
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