CN115572635A - Wear-resistant lubricating oil for drill bit and preparation method thereof - Google Patents

Wear-resistant lubricating oil for drill bit and preparation method thereof Download PDF

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CN115572635A
CN115572635A CN202211176350.4A CN202211176350A CN115572635A CN 115572635 A CN115572635 A CN 115572635A CN 202211176350 A CN202211176350 A CN 202211176350A CN 115572635 A CN115572635 A CN 115572635A
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parts
lubricating oil
stirring
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boron nitride
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李龙生
陈圣军
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Shenzhen City China Optical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04Mixtures of base-materials and additives
    • C10M169/045Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution and non-macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/061Carbides; Hydrides; Nitrides
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10Compounds containing silicon
    • C10M2201/102Silicates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • 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
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure

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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 an antiwear lubricating oil for a drill bit and a preparation method thereof, wherein the antiwear lubricating oil comprises the following components: base oil, phosphate, a stabilizer, modified sepiolite, modified boron nitride and an antioxidant antiwear agent; the wear-resistant lubricating oil is prepared by adopting a scientific proportion and a preparation method. Compared with the prior art, the anti-wear lubricating oil prepared by the invention enhances the friction lubricating property, reduces the interface thermal resistance of the lubricating oil, improves the bearing capacity of the lubricating oil, has simple and environment-friendly processing process and stable product quality, and is suitable for being used as the lubricating oil of the drill bit.

Description

Wear-resistant lubricating oil for drill bit and preparation method thereof
Technical Field
The invention relates to the technical field of lubrication, in particular to anti-wear lubricating oil for a drill bit and a preparation method thereof.
Background
In general, frictional wear is common in various aspects of daily life, which results in energy consumption in the field of mechanical engineering and affects stable operation. Therefore, the use of a lubricant to separate and lubricate two friction surfaces is one of the most effective methods of reducing friction and wear. At present, many lubricant additives, such as ionic liquids, carbon-based materials, and nanocomposite-based additives, have been synthesized to improve the tribological properties of base oils. However, lubricating oil additives have limited lubricating effectiveness under extreme conditions of high temperature, high oxygen, ultraviolet radiation, and high vacuum. In the working process of the drill bit, high heat and high friction are generated, and in order to prolong the service life of the drill bit, the research of a drill bit lubricant with high heat conduction, high wear resistance and high load resistance is very important.
The invention discloses a special transmission extreme-pressure anti-wear lubricating oil composition for a rotary drilling machine, belonging to the field of lubricant production. The composition is prepared by mixing lubricating oil base oil, a pour point depressant, an S extreme pressure anti-wear agent, an extreme pressure anti-wear agent and a system anti-variation agent. Compared with the prior art, the extreme pressure antiwear performance and the bearing capacity are high, and the method has good popularization and application values. However, the lubricating oil composition prepared by the invention has poor heat conductivity and insufficient wear resistance.
The chinese patent CN104194886B discloses an antiwear lubricating oil and a preparation method thereof, wherein the antiwear lubricating oil is composed of the following raw materials by weight: 30-60 parts of organic molybdenum, 1-5 parts of nano barium carbonate/nano aluminum compound, 20-40 parts of sulfurized whale oil, 10-30 parts of isooctyl oleate and 1-30 parts of mineral oil; in the preparation process of the nano aluminum, finished aluminum is not directly ground, but the process from aluminum chloride hexahydrate to aluminum formate to nano aluminum is carried out, so that the obtained aluminum is purer, the prepared particle size is more uniform, and the wear resistance of the aluminum is more favorable; the lubricating oil has extremely high wear resistance, and the extreme pressure performance and the long-term wear performance of the lubricating oil are greatly improved. However, the antiwear lubricating oil prepared by the invention is not suitable for lubricating a drill bit, and the lubricating property is insufficient.
Disclosure of Invention
In view of the defects of poor heat conductivity, insufficient wear resistance and insufficient load resistance of the anti-wear lubricating oil in the prior art, the technical problem to be solved by the invention is to provide the anti-wear lubricating oil for the drill bit with better heat conductivity and lubrication and the preparation method thereof.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
an antiwear lubricating oil for a drill bit comprising the following components: base oil, phosphate, a stabilizer, modified sepiolite, modified boron nitride and an antioxidant antiwear agent.
Preferably, the antiwear lubricating oil for the drill bit comprises the following components in percentage by mass: 80-90% of base oil, 2-6% of phosphate, 1-5% of stabilizer, 1-3% of modified sepiolite, 1-3% of modified boron nitride and 3-7% of antioxidant antiwear agent.
Preferably, the preparation method of the antiwear lubricating oil for drill bits is as follows: stirring and mixing the base oil, the phosphate and the stabilizer according to the formula ratio, and stirring for 30-60 min at the temperature of 60-90 ℃ and the stirring speed of 400-800 rpm to obtain a mixture; adding the modified sepiolite, the modified boron nitride and the antioxidant antiwear agent into the mixture, continuously stirring for 2-4 h at the temperature of 50-70 ℃, wherein the stirring speed is 200-400 rpm, and then cooling at normal temperature to obtain the antiwear lubricating oil.
Preferably, the base oil is at least one of a mineral lubricating oil and a synthetic lubricating oil.
Preferably, the phosphate is at least one of lauryl alcohol phosphate, alkylphenol polyoxyethylene phosphate, isooctanol polyoxyethylene monophosphate, isotridecyl alcohol phosphate and phenol polyoxyethylene phosphate.
Preferably, the stabilizer is at least one of calcium zinc stabilizer, nonyl phenol and polyoxyethylene stearate.
Preferably, the preparation method of the modified sepiolite comprises the following steps of: adding 3-8 parts of sepiolite powder into 70-100 parts of toluene, adding 0.1-0.3 part of oleic acid, stirring for 10-30 min at the stirring speed of 50-200 rpm, then adding 1-3 parts of dicyclohexylcarbodiimide and 1-5 parts of 4-dimethylaminopyridine, carrying out ball milling, centrifuging at 3000-5000 rpm for 20-50 min after the ball milling process is finished, filtering by using a 300-450-mesh sieve, and drying at 40-60 ℃ for 1-3 h to obtain the modified sepiolite.
Preferably, the ball milling parameters are that the ball milling rotating speed is 300-400 rpm, the ball milling time is 5-15 h, the grinding balls are agate beads, and the ball material ratio is 20-30.
Preferably, the preparation method of the modified boron nitride comprises the following steps of: dispersing 0.5-2 parts of boron nitride powder and 10-20 parts of tri-n-octylamine in 20-40 parts of dimethylacetamide, stirring for 20-40 min at the speed of 100-300 rpm for 20-40 min under ultrasonic power of 200-400W at the frequency of 40-60 kHz to obtain a dispersion solution, transferring the dispersion solution to a ball mill containing zirconia balls with the diameter of 3-8 mm, wherein the ball-to-material ratio is 40-60, the ball-milling speed is 300-500 rpm, the ball-milling time is 20-30 h, centrifuging the obtained solution at the rpm of 2000-4000 for 3-8 min after ball-milling, collecting supernatant, washing with 30-50 parts of dimethylacetamide for three times, and drying at the temperature of 70-90 ℃ for 20-30 h to obtain the modified boron nitride.
Preferably, the preparation method of the antioxidant antiwear agent comprises the following steps:
s1, adding 1-5 parts of lithium fluoride into 10-20 parts of water, then adding 20-40 parts of 36-38 wt% hydrochloric acid, stirring for 20-40 min at 30-50 ℃ by using a magnetic stirrer to obtain a mixed solution, slowly adding 1-3 parts of titanium aluminum carbide powder into the mixed solution, covering a layer of preservative film with small holes, reacting for 20-30 h, centrifuging the suspension at 3000-4000 rpm for 3-8 min, collecting lower-layer substances, adding water, uniformly shaking, centrifuging for 5-15 min at 8000-12000 rpm, freezing precipitates after centrifugation, and freeze-drying in vacuum for 1-3 d at the freezing temperature of-15-5 ℃ and the vacuum degree of 0.03-0.08 MPa to obtain a compound;
s2, dispersing the compound prepared in the step S1 in 150-300 parts of 3-8wt% NaOH aqueous solution, stirring for 5-10 h at the stirring speed of 100-300 rpm, centrifuging for 20-40 min at 3000-5000 rpm, freezing the precipitate, and carrying out vacuum freeze drying for 1-5 d at the freezing temperature of-15 to-5 ℃ and the vacuum degree of 0.03-0.08 MPa to obtain an alkalized compound, soaking the alkalized compound in 5-15 parts of water, carrying out ultrasonic dispersion for 1-3 h, wherein the ultrasonic power is 200-400W, and the ultrasonic frequency is 30-60 kHz to obtain an alkalized solution; then, dissolving 1-3 parts of 25-28 wt% ammonia water and 0.1-0.5 part of gamma-methacryloxypropyltrimethoxysilane in 30-50 parts of absolute ethyl alcohol to obtain a functional solution, mixing the functional solution and the alkalizing solution, stirring and reacting for 20-30 h at 40-60 ℃, wherein the stirring speed is 200-400 rpm, and then washing with absolute ethyl alcohol to obtain a precipitate;
and S3, adding the precipitate prepared in the step S2, 0.1-0.5 part of azodiisobutyronitrile and 1-5 parts of acetoacetoxyethylmethacrylate into 40-60 parts of acetonitrile, introducing helium to discharge oxygen, reacting at 70-80 ℃ for 5-10 hours, washing with absolute ethyl alcohol, and drying at room temperature to obtain the antioxidant antiwear agent.
The method comprises the steps of carrying out esterification reaction on sepiolite powder and oleic acid, and carrying out modification grinding on dicyclohexylcarbodiimide and 4-dimethylaminopyridine to prepare modified sepiolite; then modifying the boron nitride powder in dimethylacetamide by adopting tri-n-octylamine to obtain modified boron nitride; and then reacting and compounding lithium fluoride and titanium aluminum carbide to obtain a compound, alkalifying the compound, grafting the compound with gamma-methacryloxypropyltrimethoxysilane to obtain a precipitate, and reacting the precipitate with azodiisobutyronitrile and acetoacetoxy ethyl methacrylate in acetonitrile to obtain the antioxidant antiwear agent. And adding the prepared modified sepiolite, the modified boron nitride and the antioxidant antiwear agent into base oil, and mixing to obtain the antiwear lubricant. The anti-wear lubricant prepared by the invention has good friction performance, on one hand, nitrogen atoms in tri-n-octylamine molecules can interact with boron atoms on the surface of boron nitride through the action of dimethylacetamide, alkyl chains are successfully grafted with the boron nitride molecules, and the dispersion of alkylated boron nitride in mineral oil is enhanced due to the action of van der Waals force between the boron nitride alkyl chains grafted on the surface and hydrocarbon in the mineral oil, so that larger steric hindrance is formed, and the improvement of friction and thermal conductivity is facilitated. The large space potential resistance value can effectively inhibit the aggregation of particles, thereby ensuring the long-term dispersion stability of the particles in mineral oil. The grafted material is converted from oleophobic material to lipophilic material, which makes it compatible with base oil, and the ungrafted boron nitride itself is less lipophilic and undergoes agglomeration or precipitation in mineral base oil, resulting in an increase in frictional resistance. Good dispersion of the alkylated boron nitride in the base oil may promote lubrication performance. On the other hand, after the compound is alkalized, the compound is grafted with gamma-methacryloxypropyl trimethoxy silane through C = C bonds, and polymerization is initiated on the surface of acetoacetoxy ethyl methacrylate, so that the obtained antioxidant antiwear agent has excellent dispersibility, a stable lubricating film is formed by the antioxidant antiwear agent, the formed structure has good heat conductivity, the antioxidant antiwear agent and the modified boron nitride have a synergistic effect, the antioxidant antiwear agent and the modified boron nitride are uniformly dispersed in base oil, and a dispersion is formed through steric hindrance, so that the lubricating oil is endowed with appropriate viscosity, and the heat conductivity is enhanced. Further, the long-chain oleic acid is successfully grafted to the sepiolite powder through the esterification reaction of the sepiolite powder and the oleic acid, so that the modified sepiolite powder has good compatibility in the lubricating oil. The friction film formed by sepiolite in lubricating oil mainly comprises various oxides, and in the process of friction lubrication, the modified sepiolite participates in the tribochemical reaction of a friction interface, and a friction layer consisting of metal oxides and oxidized ceramics is formed on the friction surface. The ceramic phase and the metal oxide play an important role in strengthening a friction layer, the phyllosilicate mineral has strong adsorption capacity and can be quickly adsorbed and deposited on a wear surface in a friction process to grind, polish, fill and repair micro-protrusions, pits and micro-damage on the surface of a material, so that the roughness is reduced, the distribution of a stress contact surface is optimized, the friction and the wear are improved, a dispersion is formed to generate a complementary effect with an antioxidant antiwear agent and modified boron nitride, and a formed lubricating oil film can reduce the friction loss, improve the loss and enhance the friction and lubrication performance.
The lubricating oil prepared by the invention has higher oil film strength, enhanced wear resistance and effectively improved extreme pressure performance of base oil, and is mainly characterized in that the lubricating oil prepared by adding modified boron nitride, an antioxidant antiwear agent and modified sepiolite has higher heat conductivity coefficient, and an effective heat conduction path is established by the modified boron nitride and a dispersion formed by the antioxidant antiwear agent, so that the interfacial thermal resistance of the base oil can be effectively reduced, and the heat conductivity of the base oil can also be improved. The modified sepiolite can form a friction film with excellent micro-mechanical performance under local high pressure and high temperature generated in a flash state, so that sliding friction is reduced, rolling friction is increased, and the bearing capacity of lubricating oil is improved.
Compared with the prior art, the invention has the beneficial effects that:
1) The invention carries out esterification reaction on sepiolite powder and oleic acid, and modified sepiolite is prepared by modifying and grinding dicyclohexylcarbodiimide and 4-dimethylamino pyridine; then modifying the boron nitride powder in dimethylacetamide by adopting tri-n-octylamine to obtain modified boron nitride; and then reacting and compounding lithium fluoride and titanium aluminum carbide to obtain a compound, alkalifying the compound, grafting the compound with gamma-methacryloxypropyltrimethoxysilane to obtain a precipitate, and reacting the precipitate with azodiisobutyronitrile and acetoacetoxy ethyl methacrylate in acetonitrile to obtain the antioxidant antiwear agent. The prepared modified sepiolite, modified boron nitride and the antioxidant antiwear agent are added into base oil and mixed to obtain an antiwear lubricant, so that the friction lubrication performance is enhanced, the interface thermal resistance of the base oil is reduced, and the bearing capacity of the lubricating oil is improved;
2) The wear-resistant lubricating oil is prepared by adopting a scientific proportion and a preparation method, the processing process is simple and environment-friendly, the product quality is stable, and the additive has good dispersibility and is suitable for being used as the lubricating oil of the drill bit.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
The parameters of part of the raw materials in the embodiment of the invention are as follows:
sepiolite powder, new materials, inc, of hunan, china. The purity of the powder is 97.3 percent, and the average grain diameter is 0.7-1.1 um;
base oil, shenzhen china Huamei lubricating science and technology Limited, model: 100N, kinematic viscosity at 40 ℃:19.5mm 2 S, viscosity index: 124;
4-dimethylaminopyridine, shandong Huayao Biotech, inc., cat #: 123, CAS:1122-58-3;
lauryl alcohol phosphate, a heian petrochemical plant of Jiangsu province, type: MA24P, appearance (visual inspection at 25 ℃): white to light yellow cream block;
calcium zinc stabilizer, reed chemical technology ltd, fujian province, cat #: 0227, content of effective substances: 99 percent;
boron nitride powder, shandong Liang New Material science and technology Limited, model: LA-8Q, CAS:10043-11-5;
tri-n-octylamine, shanghai kinoform biotechnology limited, content: 99%, appearance: powder, color: light yellow;
lithium fluoride, baodinafosite new materials ltd, molecular weight: 25.94, CAS:7789-24-4;
titanium aluminum carbide powder, shanghai nahmi nanotechnology limited, content not less than 99.9%, particle size: 325/1000 mesh;
gamma-methacryloxypropyltrimethoxysilane, guangzhou, new materials ltd, cat No.: 01, CAS:2530-85-0.
Example 1
An antiwear lubricating oil for drill bits is prepared by the following steps:
85kg of 100N base oil (viscosity index: 124, content of saturated hydrocarbon: 96 wt%), 4kg of lauryl phosphate and 3kg of calcium-zinc stabilizer were mixed by stirring, and stirred at 80 ℃ for 40min at a stirring speed of 600rpm to obtain a mixture; adding 2kg of modified sepiolite, 2kg of modified boron nitride and 4kg of antioxidant antiwear agent into the mixture, continuously stirring for 2.5h at the temperature of 60 ℃, wherein the stirring speed is 300rpm, and then cooling at normal temperature to obtain the antiwear lubricating oil.
The preparation method of the modified sepiolite comprises the following steps:
adding 5kg of sepiolite powder into 95kg of toluene, adding 0.2kg of oleic acid, stirring for 20min at the stirring speed of 100rpm, then adding 2kg of dicyclohexylcarbodiimide and 3kg of 4-dimethylaminopyridine, processing by adopting a high-energy ball mill at the rotation speed of 350rpm for 10h, wherein the grinding balls are agate balls, the ball-to-material ratio is 25:1, and after the ball-milling process is finished, centrifuging for 30min at 4000rpm, filtering by a 400-mesh sieve, and drying for 2h at 50 ℃ to obtain the modified sepiolite.
The preparation method of the modified boron nitride comprises the following steps:
dispersing 1kg of boron nitride powder and 15.5kg of tri-n-octylamine in 30kg of dimethylacetamide, stirring for 30min at the stirring speed of 200rpm and the ultrasonic power of 300W at the ultrasonic frequency of 50kHz to obtain a dispersion solution, then transferring the dispersion solution to a ball mill containing zirconia balls with the diameter of 5mm to obtain a ball-mill with the ball-to-material ratio of 50.
The preparation method of the antioxidant antiwear agent comprises the following steps:
s1, adding 3kg of lithium fluoride into 15kg of water, then adding 30kg of 37wt% hydrochloric acid, stirring for 30min at 40 ℃ by using a magnetic stirrer to obtain a mixed solution, slowly adding 2kg of titanium aluminum carbide powder into the mixed solution, covering a layer of preservative film with small holes, reacting for 24h, centrifuging suspension at 3500rpm for 5min, collecting lower-layer substances, adding water, shaking uniformly, centrifuging at 10000rpm for 10min, freezing precipitates after centrifugation, and freeze-drying in vacuum for 2d at the freezing temperature of-10 ℃ and the vacuum degree of 0.05MPa to obtain a compound;
s2, dispersing the compound prepared in the step S1 in 200kg of 5wt% NaOH aqueous solution, stirring for 8 hours at a stirring speed of 200rpm, centrifuging at 4000rpm for 30 minutes, freezing the precipitate, and carrying out vacuum freeze drying for 3d at a freezing temperature of-10 ℃ and a vacuum degree of 0.05MPa to obtain an alkalized compound, soaking the alkalized compound in 10kg of water, and carrying out ultrasonic dispersion for 2 hours at an ultrasonic power of 300W and an ultrasonic frequency of 50kHz to obtain an alkalized solution; then, dissolving 1.5kg of 27wt% ammonia water and 0.3kg of gamma-methacryloxypropyltrimethoxysilane in 40kg of absolute ethyl alcohol to obtain a functional solution, mixing the functional solution and the alkalized solution, stirring and reacting for 24 hours at 50 ℃, wherein the stirring speed is 300rpm, and then washing with absolute ethyl alcohol to obtain a precipitate;
and S3, adding the precipitate prepared in the step S2, 0.35kg of azodiisobutyronitrile and 2kg of acetoacetoxyethylmethacrylate into 50kg of acetonitrile, introducing helium to discharge oxygen, reacting at 75 ℃ for 8h, finally washing with absolute ethanol, and drying at room temperature to obtain the antioxidant antiwear agent.
Example 2
An antiwear lubricating oil for a drill bit was prepared in substantially the same manner as in example 1, with the only difference being that: the preparation methods of the antiwear lubricating oil for the drill bit are different.
The preparation method of the anti-wear lubricating oil for the drill bit comprises the following steps:
85kg of 100N base oil (viscosity index: 124, content of saturated hydrocarbon: 96 wt%), 4kg of lauryl phosphate and 3kg of calcium-zinc stabilizer were mixed by stirring, and stirred at 80 ℃ for 40min at a stirring speed of 600rpm to obtain a mixture; adding 2kg of modified boron nitride and 4kg of antioxidant antiwear agent into the mixture, continuously stirring for 2.5h at the temperature of 60 ℃, wherein the stirring speed is 300rpm, and then cooling at normal temperature to obtain the antiwear lubricating oil.
The preparation method of the modified boron nitride is the same as that of the embodiment 1.
The preparation method of the antioxidant antiwear agent is the same as that of the example 1.
Example 3
An antiwear lubricating oil for a drill bit was prepared in substantially the same manner as in example 1, with the only difference being that: the preparation methods of the antiwear lubricating oil for the drill bit are different.
The preparation method of the antiwear lubricating oil for the drill bit comprises the following steps:
85kg of 100N base oil (viscosity index of 124, content of saturated hydrocarbon of 96 wt%), 4kg of lauryl phosphate and 3kg of calcium-zinc stabilizer were stirred and mixed, and stirred at 80 ℃ for 40min at a stirring speed of 600rpm to obtain a mixture; adding 2kg of modified sepiolite and 4kg of antioxidant antiwear agent into the mixture, continuously stirring for 2.5h at the temperature of 60 ℃, wherein the stirring speed is 300rpm, and then cooling at normal temperature to obtain the antiwear lubricating oil.
The preparation method of the modified sepiolite is the same as that of the example 1.
The preparation method of the antioxidant antiwear agent is the same as that of the example 1.
Example 4
An antiwear lubricating oil for a drill bit was prepared in substantially the same manner as in example 1, with the only difference being that: the preparation methods of the antiwear lubricating oil for the drill bit are different.
The preparation method of the antiwear lubricating oil for the drill bit comprises the following steps:
85kg of 100N base oil (viscosity index: 124, content of saturated hydrocarbon: 96 wt%), 4kg of lauryl phosphate and 3kg of calcium-zinc stabilizer were mixed by stirring, and stirred at 80 ℃ for 40min at a stirring speed of 600rpm to obtain a mixture; adding 2kg of modified sepiolite and 2kg of modified boron nitride into the mixture, continuously stirring for 2.5h at the temperature of 60 ℃, wherein the stirring speed is 300rpm, and then cooling at normal temperature to obtain the anti-wear lubricating oil.
The preparation method of the modified sepiolite is the same as that of the example 1.
The preparation method of the modified boron nitride is the same as that of the embodiment 1.
Comparative example 1
An antiwear lubricating oil for a drill bit was prepared in substantially the same manner as in example 1, with the only difference being that: replacing the modified sepiolite by sepiolite with equal quantity and size.
Comparative example 2
An antiwear lubricating oil for a drill bit was prepared in substantially the same manner as in example 1, with the only difference being that: and replacing the modified boron nitride with equal amount and size of boron nitride.
Comparative example 3
An antiwear lubricating oil for drill bits is prepared substantially the same as in example 1, with the only difference being that: the preparation methods of the antiwear lubricating oil for the drill bit are different.
The preparation method of the anti-wear lubricating oil for the drill bit comprises the following steps:
85kg of 100N base oil (viscosity index of 124, content of saturated hydrocarbon of 96 wt%), 4kg of lauryl phosphate and 3kg of calcium-zinc stabilizer were mixed by stirring, stirred at 80 ℃ for 40min at a stirring speed of 600rpm, and then cooled at normal temperature to obtain antiwear lubricating oil.
Test example 1
Test for Friction Properties
The friction performance of the antiwear lubricating oil samples prepared according to the present invention was tested using a four-ball friction wear tester. The test is carried out according to GB/T12583-1998 four-ball method for extreme pressure performance of lubricant, the steel ball used is 12.7mm (GCr 15, 10 grade) steel ball produced by Shanghai steel ball factory under normal temperature condition, and the steel ball is immersed into absolute ethyl alcohol for ultrasonic cleaning to remove stains on the surface of the steel ball before the test. Experiment the friction Coefficient (COF) values were recorded for 10min, 30min, 60min at 1200rpm and 392N load, respectively. Each sample was tested in triplicate under identical conditions and the final results were averaged over triplicates. The test results are shown in Table 1.
Table 1: results of the Friction Performance test
Figure BDA0003864586150000101
Figure BDA0003864586150000111
(the lower the COF value, the better the drag reduction effect)
As can be seen from the test results in table 1, example 1 has the best friction performance, probably because the modified sepiolite is prepared by esterification reaction of sepiolite powder and oleic acid and modified grinding of dicyclohexylcarbodiimide and 4-dimethylaminopyridine; then modifying the boron nitride powder in dimethylacetamide by adopting tri-n-octylamine to obtain modified boron nitride; and then reacting and compounding lithium fluoride and titanium aluminum carbide to obtain a compound, alkalifying the compound, grafting the compound with gamma-methacryloxypropyltrimethoxysilane to obtain a precipitate, and reacting the precipitate with azodiisobutyronitrile and acetoacetoxy ethyl methacrylate in acetonitrile to obtain the antioxidant antiwear agent. And adding the prepared modified sepiolite, the modified boron nitride and the antioxidant antiwear agent into base oil, and mixing to obtain the antiwear lubricant. The anti-wear lubricant prepared by the invention has good friction performance, on one hand, nitrogen atoms in tri-n-octylamine molecules can interact with boron atoms on the surface of boron nitride through the action of dimethylacetamide, alkyl chains are successfully grafted with the boron nitride molecules, and the dispersion of alkylated boron nitride in mineral oil is enhanced due to the action of van der Waals force between the surface-grafted nitrogen boride alkyl chains and hydrocarbons in the mineral oil, so that larger steric hindrance is formed, and the improvement of friction and thermal conductivity is facilitated. The large space potential resistance value can effectively inhibit the aggregation of particles, thereby ensuring the long-term dispersion stability of the particles in mineral oil. The grafted material is converted from an oleophobic material to a lipophilic material, making it compatible with the base oil, the ungrafted boron nitride itself is less lipophilic and agglomerates or precipitates in the mineral base oil, resulting in an increase in frictional resistance. Good dispersion of the alkylated boron nitride in the base oil may promote lubrication performance. After the compound is alkalized, the compound is grafted with gamma-methacryloxypropyltrimethoxysilane by forming a C = C bond, and the acetoacetoxy ethyl methacrylate is subjected to surface initiated polymerization to obtain the antioxidant antiwear agent which also has excellent dispersibility. Further, the long-chain oleic acid is successfully grafted to the sepiolite powder through the esterification reaction of the sepiolite powder and the oleic acid, so that the modified sepiolite powder has good compatibility in the lubricating oil. The friction film formed by sepiolite in lubricating oil mainly comprises various oxides, and in the process of friction lubrication, the modified sepiolite participates in the tribochemical reaction of a friction interface, and a friction layer consisting of metal oxides and oxidized ceramics is formed on the friction surface. The ceramic phase and the metal oxide play an important role in strengthening a friction layer, the phyllosilicate mineral has strong adsorption capacity, can be quickly adsorbed and deposited on a wear surface in a friction process, and can grind, polish, fill and repair micro-protrusions, pits and micro-damage on the surface of a material, so that the roughness is reduced, the distribution of a stress contact surface is optimized, the improvement of friction and wear is facilitated, a dispersion body formed by the phyllosilicate mineral, an anti-wear agent and modified boron nitride has a complementary effect, and a formed lubricating oil film can reduce friction loss, improve loss and enhance friction and lubrication performance.
Test example 2
Bearing capacity test
The load bearing capacity of the lubricating oil was tested. The extreme pressure bearing capacity, i.e. the maximum non-seizure load value P, of the lubricating oils of examples and comparative examples was tested using a (MRS-10P) hydraulic four-ball friction tester by referring to GB/T3142-2019 "lubricating oil bearing capacity determination four-ball method B
The test parameters are: the load was selected according to the test results with reference to a standard, with a rotation rate of 1450r/min and a time of 10s. Each sample was tested 3 times and the average was taken.
The test results are shown in table 2.
Table 2: bearing capacity test results
Figure BDA0003864586150000121
Figure BDA0003864586150000131
As can be seen from the test results shown in table 2, the best load-bearing capability test result in example 1 indicates that the lubricating oil prepared in example 1 of the present invention has high oil film strength, enhanced wear resistance, and effectively improved extreme pressure properties of the base oil, probably because the lubricating oil prepared by adding the modified boron nitride, the antioxidant antiwear agent, and the modified sepiolite in the present invention has a high thermal conductivity, and an effective thermal conductivity path is established with the dispersion formed by the antioxidant antiwear agent, so that the interfacial thermal resistance of the base oil can be effectively reduced, and the thermal conductivity of the base oil can also be improved. The modified sepiolite can form a friction film with excellent micro-mechanical performance under local high pressure and high temperature generated in a flash state, so that sliding friction is reduced, rolling friction is increased, and the bearing capacity of lubricating oil is improved.

Claims (10)

1. An anti-wear lubricating oil for a drill bit, comprising the following components: base oil, phosphate, a stabilizer, modified sepiolite, modified boron nitride and an antioxidant antiwear agent.
2. The anti-wear lubricating oil for drill bits according to claim 1, comprising the following components in mass percent: 80-90% of base oil, 2-6% of phosphate, 1-5% of stabilizer, 1-3% of modified sepiolite, 1-3% of modified boron nitride and 3-7% of antioxidant antiwear agent.
3. A method of preparing the antiwear lubricating oil for a drill bit according to claim 1 or 2, characterized by: stirring and mixing the base oil, the phosphate and the stabilizer according to the formula ratio, and stirring for 30-60 min at the temperature of 60-90 ℃ and the stirring speed of 400-800 rpm to obtain a mixture; adding the modified sepiolite, the modified boron nitride and the antioxidant antiwear agent into the mixture, continuously stirring for 2-4 h at the temperature of 50-70 ℃, wherein the stirring speed is 200-400 rpm, and then cooling at normal temperature to obtain the antiwear lubricating oil.
4. The method of claim 3, wherein: the base oil is at least one of mineral lubricating oil and synthetic lubricating oil.
5. The method of claim 3, wherein: the phosphate is at least one of lauryl alcohol phosphate, alkylphenol polyoxyethylene ether phosphate, isooctanol polyoxyethylene ether monophosphate, isotridecyl alcohol phosphate and phenol polyoxyethylene ether phosphate.
6. The method of claim 3, wherein: the stabilizer is at least one of calcium zinc stabilizer, nonyl phenol and polyoxyethylene stearate.
7. The method according to claim 3, wherein the modified sepiolite is prepared by the following method, wherein the parts are all parts by weight: adding 3-8 parts of sepiolite powder into 70-100 parts of toluene, adding 0.1-0.3 part of oleic acid, stirring for 10-30 min at the stirring speed of 50-200 rpm, then adding 1-3 parts of dicyclohexylcarbodiimide and 1-5 parts of 4-dimethylaminopyridine, carrying out ball milling, centrifuging at 3000-5000 rpm for 20-50 min after the ball milling process is finished, filtering by using a 300-450-mesh sieve, and drying at 40-60 ℃ for 1-3 h to obtain the modified sepiolite.
8. The method of claim 7, wherein: the ball milling parameters are that the ball milling rotating speed is 300-400 rpm, the ball milling time is 5-15 h, the grinding balls are agate beads, and the ball material ratio is 20-30: 1.
9. The method of claim 3, wherein the modified boron nitride is prepared by the following steps in parts by weight: dispersing 0.5-2 parts of boron nitride powder and 10-20 parts of tri-n-octylamine in 20-40 parts of dimethylacetamide, stirring for 20-40 min at a stirring speed of 100-300 rpm for 20-40 min under ultrasonic power of 200-400W at an ultrasonic frequency of 40-60 kHz to obtain a dispersion solution, transferring the dispersion solution to a ball mill containing zirconia balls with the diameter of 3-8 mm, wherein the ball-to-material ratio is 40-60.
10. The method of claim 3, wherein the antioxidant antiwear agent is prepared by the following method, wherein the parts are all parts by weight:
s1, adding 1-5 parts of lithium fluoride into 10-20 parts of water, then adding 20-40 parts of 36-38 wt% hydrochloric acid, stirring for 20-40 min at 30-50 ℃ by using a magnetic stirrer to obtain a mixed solution, slowly adding 1-3 parts of titanium aluminum carbide powder into the mixed solution, covering a layer of preservative film with small holes, reacting for 20-30 h, centrifuging the suspension at 3000-4000 rpm for 3-8 min, collecting the lower-layer substance, adding water, uniformly shaking, centrifuging for 5-15 min at 8000-12000 rpm, freezing the precipitate after centrifugation, and freeze-drying in vacuum for 1-3 d at the freezing temperature of-15-5 ℃ and the vacuum degree of 0.03-0.08 MPa to obtain a compound;
s2, dispersing the compound prepared in the step S1 in 150-300 parts of 3-8wt% NaOH aqueous solution, stirring for 5-10 h at the stirring speed of 100-300 rpm, centrifuging for 20-40 min at 3000-5000 rpm, freezing the precipitate, and carrying out vacuum freeze drying for 1-5 d at the freezing temperature of-15 to-5 ℃ and the vacuum degree of 0.03-0.08 MPa to obtain an alkalized compound, soaking the alkalized compound in 5-15 parts of water, carrying out ultrasonic dispersion for 1-3 h, wherein the ultrasonic power is 200-400W, and the ultrasonic frequency is 30-60 kHz to obtain an alkalized solution; then, dissolving 1-3 parts of 25-28 wt% ammonia water and 0.1-0.5 part of gamma-methacryloxypropyltrimethoxysilane in 30-50 parts of absolute ethyl alcohol to obtain a functional solution, mixing the functional solution and the alkalizing solution, stirring and reacting for 20-30 h at 40-60 ℃, wherein the stirring speed is 200-400 rpm, and then washing with absolute ethyl alcohol to obtain a precipitate;
and S3, adding the precipitate prepared in the step S2, 0.1-0.5 part of azodiisobutyronitrile and 1-5 parts of acetoacetoxy ethyl methacrylate into 40-60 parts of acetonitrile, introducing helium to discharge oxygen, reacting at 70-80 ℃ for 5-10 h, washing with absolute ethyl alcohol, and drying at room temperature to obtain the antioxidant antiwear agent.
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