CN110819423A - Alkene alloy lubricating oil additive and processing technology thereof - Google Patents

Alkene alloy lubricating oil additive and processing technology thereof Download PDF

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CN110819423A
CN110819423A CN201910972775.8A CN201910972775A CN110819423A CN 110819423 A CN110819423 A CN 110819423A CN 201910972775 A CN201910972775 A CN 201910972775A CN 110819423 A CN110819423 A CN 110819423A
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parts
modified
mixing
graphene oxide
placing
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袁国祥
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Jiangsu Dipaene Alloy Technology Co Ltd
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Jiangsu Dipaene Alloy Technology Co Ltd
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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
    • C10M167/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound, a non-macromolecular compound and a compound of unknown or incompletely defined constitution, each of these compounds being essential
    • 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
    • C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/05—Metals; Alloys
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/082—Inorganic acids or salts thereof containing nitrogen
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085—Phosphorus oxides, acids or salts
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—Hydroxy compounds
    • C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/022—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/04—Ethers; Acetals; Ortho-esters; Ortho-carbonates
    • C10M2207/046—Hydroxy ethers
    • 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
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/042—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds between the nitrogen-containing monomer and an aldehyde or ketone
    • 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
    • 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

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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 relates to the technical field of oil additives, in particular to an olefin alloy lubricating oil additive and a processing technology thereof. Mixing pretreated graphene oxide, absolute ethyl alcohol, nano titanium powder and nano silver powder, heating, ball milling, filling chlorine gas, pressurizing, reacting at constant temperature, heating, exhausting, heating step by step, adding molybdenum disulfide, filling nitrogen gas for reacting, cooling, adding rare earth, stirring at constant temperature for reacting, exhausting, adding sodium thiosulfate, cooling, stirring to room temperature, drying to obtain modified graphene oxide, mixing furfurylamine, terephthalaldehyde and cardanol, stirring at constant temperature for reacting, performing rotary evaporation and concentration to obtain modified resin, mixing the modified multi-walled carbon nanotube and the modified graphene oxide, ball milling, adding the modified resin, calcium nitrate, polyalcohol and phospholipid, and ball milling and mixing to obtain the alkene alloy lubricating oil additive. The alkene alloy lubricating oil additive provided by the invention has excellent wear resistance.

Description

Alkene alloy lubricating oil additive and processing technology thereof
Technical Field
The invention relates to the technical field of oil additives, in particular to an olefin alloy lubricating oil additive and a processing technology thereof.
Background
The lubricating oil mainly consists of base oil and additives, wherein the base oil is a main component which plays the main role of the lubricating oil, and the development requirements of the current engine technology are difficult to meet by changing the traditional petroleum refining method, so the use of the additives becomes the best choice. The additive is used for making up for the deficiency of certain properties of the traditional lubricating oil, and the effect is obvious although the addition amount is small. The additive accounts for less than 10% of the general industrial lubricating oil, the additive components of the internal combustion engine oil account for about 20%, and the additive can account for more than 30% of the high-base-number marine cylinder oil.
Through a large number of experiments, research personnel find out the optimal combination of various additives, so that the lubricant can reach the specific performance and save the addition amount, which is a key index for judging the quality of the lubricating oil. For the mainstream brand lubricating oil in the current market, the quality difference of the base oil is smaller and smaller, and the main difference lies in the use of the additive, and the variety, type, dosage and formula of the additive in different finished oils are different. Because of the rigorous requirements of modern processing and production, the abrasion of the staggered parts of the parts is intensified, and the lubricating oil added to the parts is gradually unable to keep pace with the development in performance. Therefore, research can be carried out in the direction of lubricating oil additives to improve the anti-wear performance of the additives.
Disclosure of Invention
The invention aims to provide an olefin alloy lubricating oil additive and a processing technology thereof, and aims to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the alkene alloy lubricating oil additive comprises the following raw materials in parts by weight: 8-10 parts of modified multi-walled carbon nanotubes, 10-20 parts of modified graphene oxide, 10-20 parts of modified resin, 10-20 parts of polyhydric alcohol, 1-2 parts of calcium nitrate and 8-10 parts of phospholipid.
The polyhydric alcohol is any one of diethylene glycol, dipropylene glycol or trimethylolpropane.
The phospholipid is any one of soybean phospholipid, yolk phospholipid or peanut phospholipid.
The modified multi-walled carbon nanotube comprises the following raw materials in parts by weight: 3-5 parts of multi-walled carbon nanotubes, 50-60 parts of sulfuric acid solution and 8-10 parts of nitric acid solution.
The modified graphene oxide comprises the following raw materials in parts by weight: 20-30 parts of pretreated graphene oxide, 20-30 parts of absolute ethyl alcohol, 3-5 parts of molybdenum disulfide, 20-30 parts of nano titanium powder and 10-20 parts of nano silver powder.
The pretreated graphene oxide comprises the following raw materials in parts by weight: 30-40 parts of graphene oxide, 10-20 parts of modified fullerene, 1-2 parts of hydrazine hydrate, 60-80 parts of water and 20-30 parts of dimethyl sulfoxide.
The modified resin comprises the following raw materials in parts by weight: 10-20 parts of furfuryl amine, 8-10 parts of terephthalaldehyde and 20-30 parts of cardanol.
The alkene alloy lubricating oil additive comprises the following raw materials in parts by weight: 10 parts of modified multi-walled carbon nanotube, 20 parts of modified graphene oxide, 20 parts of modified resin, 20 parts of polyol, 2 parts of calcium nitrate and 10 parts of phospholipid.
A processing technology of an olefin alloy lubricating oil additive comprises the following specific preparation steps:
(1) processing the multi-walled carbon nanotubes;
(2) pretreating graphene oxide;
(3) modifying the product obtained in the step (2);
(4) preparing modified resin;
(5) mixing materials;
(6) and (6) detecting.
The processing steps of the alkene alloy lubricating oil additive are as follows:
(1) mixing a sulfuric acid solution and a nitric acid solution, adding a multi-walled carbon nanotube, stirring for reaction, filtering, washing and drying to obtain a modified multi-walled carbon nanotube, wherein in the preparation process, the multi-walled carbon nanotube is treated by mixed acid to enable the surface of the multi-walled carbon nanotube to contain a large number of oxygen-containing groups, and in the use process, the modified multi-walled carbon nanotube can be combined with hydrophilic groups on the surface of modified graphene oxide, so that the oil solubility of the modified graphene oxide can be effectively improved, the graphene oxide can be well dispersed in a system, and the wear resistance of a product can be further improved;
(2) mixing graphene oxide with water and ultrasonically treating to obtain No. 1 dispersion liquid, mixing modified fullerene with dimethyl sulfoxide and ultrasonically treating to obtain No. 2 dispersion liquid, stirring and mixing the No. 1 dispersion liquid and the No. 2 dispersion liquid, adding hydrazine hydrate, heating for reaction, cooling and centrifuging, filtering, washing and drying to obtain pretreated graphene oxide, wherein in the use process, the ultrathin lamellar structure of the graphene oxide enables the graphene oxide to easily enter a contact surface to reduce the direct contact of a rough surface, due to the hollow spherical structure of the fullerene, the modified fullerene can inhibit the agglomeration of the graphene oxide, can increase the sliding effect of two contact surfaces attached to the middle of the graphene oxide lamellar layer, forms a lubricating film on the friction surface to improve the antifriction performance of the lubricating oil, and the spherical fullerene ball structure has good elasticity to effectively block the contact of the friction surface, the abrasion resistance of the product is further improved;
(3) mixing the pretreated graphene oxide, absolute ethyl alcohol, nano titanium powder and nano silver powder, heating, ball milling, filling chlorine, pressurizing, reacting at constant temperature, heating, exhausting, heating step by step, adding molybdenum disulfide, filling nitrogen for reacting, cooling, adding rare earth, stirring at constant temperature for reacting, exhausting, adding sodium thiosulfate, cooling, stirring to room temperature, and drying to obtain modified graphene oxide;
(4) mixing furfuryl amine, terephthalaldehyde and cardanol, stirring at constant temperature for reaction, performing rotary evaporation and concentration to obtain modified resin, performing ring opening and polymerization on a five-membered ring of furfuryl amine in the preparation process, so that the crosslinking density of matrix resin is increased, internal crosslinking networks are increased, the mechanical property and the heat resistance of a product are effectively improved, and in the use process, the polymerized resin can be filled with alkene alloy in a system and damage to the surface of the polymerized resin and firmly attached to the surface of a machine, so that the wear resistance of the system is further improved;
(5) mixing and ball-milling the modified multi-walled carbon nanotube and the modified graphene oxide, adding the modified resin, calcium nitrate, polyol and phospholipid, and ball-milling and mixing to obtain the alkene alloy lubricating oil additive, wherein in the use process of the alkene alloy lubricating oil additive, the phospholipid can be decomposed at high temperature in a system, the decomposed polyphosphoric acid can be combined with calcium ions in the system to form calcium hydroxy phosphate, and the obtained calcium hydroxy phosphate is attached to the damage of the friction surface, so that the damage of the friction surface can be effectively repaired, and the wear resistance of the product is further improved;
(6) and (6) detecting.
The processing process of the alkene alloy lubricating oil additive is as follows:
(1) putting a nitric acid solution with the mass fraction of 68% into a beaker, slowly pouring a sulfuric acid solution with the mass fraction of 70% into concentrated nitric acid along the wall of the beaker, mixing while stirring, adding a multi-walled carbon nanotube into the beaker, stirring and reacting for 40-60 min at the rotation speed of 400-500 r/min, filtering to obtain filter residue, washing the filter residue with ammonia water with the mass fraction of 20-30% until the washing liquid is neutral, then putting the washed filter residue into an oven, and drying at the temperature of 105-110 ℃ to constant weight to obtain the modified multi-walled carbon nanotube;
(2) placing graphene oxide and water into a No. 1 single-neck flask, placing a three-neck flask into an ultrasonic disperser, mixing ultrasonic waves for 40-60 min under the condition that the ultrasonic frequency is 55-75 kHz to obtain No. 1 dispersion liquid, placing modified fullerene and dimethyl sulfoxide into a No. 2 single-neck flask, placing the three-neck flask into the ultrasonic disperser, mixing ultrasonic waves for 40-60 min under the condition that the ultrasonic frequency is 55-75 kHz to obtain No. 2 dispersion liquid, placing the No. 1 dispersion liquid and the No. 2 dispersion liquid into a hydrothermal reaction kettle, stirring and mixing for 10-30 min under the condition that the rotating speed is 300-500 r/min, adding hydrazine hydrate into the hydrothermal reaction kettle, heating and reacting for 6-8 h under the condition that the temperature is 96-98 ℃, cooling and centrifuging to obtain mixed liquid, filtering the mixed liquid to obtain filter cakes, washing the filter cakes for 5-8 times by using absolute ethyl alcohol, then, placing the filter cake in an oven, and drying for 40-60 min to obtain pretreated graphene oxide;
(3) mixing pretreated graphene oxide, absolute ethyl alcohol, nano titanium powder and nano silver powder, placing the mixture in a ball mill, heating and ball milling for 40-60 min at the temperature of 200-220 ℃ to obtain a ball grinding material, then placing the ball grinding material in an alloy furnace, filling chlorine gas into the alloy furnace at the speed of 60-90 mL/min, pressurizing and reacting at the pressure of 12-15 MPa and the temperature of 200-220 ℃ for 30-50 min, heating to the temperature of 420 ℃, carrying out constant temperature treatment for 1-2 h, exhausting, heating to the temperature of 1100-1200 ℃ at the speed of 10-15 ℃/min, then adding molybdenum disulfide into the alloy furnace, filling nitrogen gas into the alloy furnace at the speed of 60-90 mL/min, stirring and reacting at the temperature of 1100-1200 ℃ for 5-8 h, cooling to 320-350 ℃, then adding rare earth into the alloy furnace, adding rare earth into the alloy furnace at the temperature of 320-350 ℃, stirring at constant temperature for reaction for 2-3 h, exhausting, adding sodium thiosulfate, cooling and stirring to room temperature, discharging to obtain a treated material, placing the treated material in an oven, and drying at 105-110 ℃ for 40-60 min to obtain modified graphene oxide;
(4) placing furfuryl amine, terephthalaldehyde and cardanol into a four-neck flask, then placing the four-neck flask into a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 40-60 min at a constant temperature under the conditions that the temperature is 65-70 ℃ and the rotating speed is 500-800 r/min to obtain mixed slurry, then placing the mixed slurry into a rotary evaporator, and performing rotary evaporation and concentration for 40-60 min under the conditions that the temperature is 60-65 ℃ to obtain modified resin;
(5) placing the modified multi-walled carbon nanotube and the modified graphene oxide in a ball mill, mixing and ball-milling for 40-60 min, adding modified resin, calcium nitrate, polyol and phospholipid, and ball-milling and mixing for 40-60 min to obtain the alkene alloy lubricating oil additive;
(6) and (6) detecting.
The preparation steps of the modified fullerene in the step (2) are as follows:
(1) sequentially taking 1-2 parts of fullerene C by weight60100-200 parts of ethylenediamine, 100-200 parts of acetone, 20-30 parts of distilled water, and mixing the fullerene C60Putting ethylenediamine and the mixture into a reactor, introducing nitrogen into the reactor at a rate of 60-90 mL/min, reacting for 40-60 min at a temperature of 80-82 ℃ and a rotation speed of 600-800 r/min to obtain mixed slurry, putting the mixed slurry into a rotary evaporator, carrying out reduced pressure rotary evaporation for 40-60 min at a temperature of 60-70 ℃ to obtain concentrated solution, mixing the concentrated solution with distilled water, adding acetone, diluting and crystallizing for 18-24 h, and filtering to obtain pretreated fullerene;
(2) taking 1-2 parts by weight of pretreated fullerene, 20-30 parts by weight of water and 5-8 parts by weight of 65% nitric acid in sequence, placing the pretreated fullerene and the water in a No. 3 single-neck flask, stirring and mixing for 40-60 min at the rotating speed of 400-600 r/min, adding the nitric acid, placing the No. 3 single-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 1-2 h at the temperature of 26-30 ℃ and the rotating speed of 600-800 r/min to obtain a mixed treatment liquid, placing the mixed treatment liquid in a rotary evaporator, decompressing and carrying out rotary evaporation for 40-60 min at the temperature of 70-80 ℃ to obtain concentrated slurry, placing the concentrated slurry in a vacuum drier, and drying to constant weight to obtain the modified fullerene.
Compared with the prior art, the invention has the beneficial effects that:
(1) in the preparation process, after the multi-walled carbon nanotube is treated by mixed acid, the surface of the multi-walled carbon nanotube contains a large number of oxygen-containing groups, and in the use process, the modified multi-walled carbon nanotube can combine with and shield hydrophilic groups on the surface of the modified graphene oxide, so that the oil solubility of the modified graphene oxide can be effectively improved, the graphene oxide can be well dispersed in a system, and the wear resistance of a product can be further improved;
(2) according to the invention, by adding the modified graphene oxide, in the use process, firstly, the ultrathin lamellar structure of the graphene oxide is easy to enter a contact surface, so that the direct contact of a rough surface is reduced; secondly, due to the hollow spherical structure of the fullerene, the modified fullerene can inhibit the agglomeration of the graphene oxide, and can increase the sliding action of two contact surfaces when attached to the middle of a graphene oxide sheet layer, so that a lubricating film is formed on the friction surface, and the antifriction performance of the lubricating oil is improved; moreover, the spherical fullerene ball structure has good elasticity, and can further effectively block the contact of the friction surface, so that the abrasion resistance of the product is further improved;
(3) in the preparation process, ring opening and polymerization are carried out on the five-membered ring of the furfuryl amine, so that the crosslinking density of matrix resin can be increased, and internal crosslinking networks are increased, so that the mechanical property and the heat resistance of the product are effectively improved;
(4) according to the invention, by adding calcium nitrate and phospholipid, in the using process, the phospholipid can be decomposed at high temperature in the system, the decomposed polyphosphoric acid can be combined with calcium ions in the system to form calcium hydroxy phosphate, and the obtained calcium hydroxy phosphate is attached to the damage of the friction surface, so that the damage of the friction surface can be effectively repaired, and the wear resistance of the product is further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
To more clearly illustrate the method of the present invention, the following examples are given, and the test methods for each index of the olefinic alloy lubricating oil additive prepared in the following examples are as follows:
the abrasion resistance (i.e. the wear-scar diameter of the steel ball, referred to as WSD for short) and the acid value are detected by a four-ball machine and a potentiometric titrator according to GB/T7304.
Example 1
The alkene alloy lubricating oil additive comprises the following raw materials in parts by weight: 10 parts of modified multi-walled carbon nanotube, 20 parts of modified graphene oxide, 20 parts of modified resin, 20 parts of polyol, 2 parts of calcium nitrate and 10 parts of phospholipid.
The polyhydric alcohol is diethylene glycol.
The phospholipid is soybean phospholipid.
The processing technology of the alkene alloy lubricating oil additive comprises the following processing steps:
(1) according to the weight parts, sequentially taking 5 parts of multi-walled carbon nanotubes, 60 parts of sulfuric acid solution and 10 parts of nitric acid solution, placing the nitric acid solution with the mass fraction of 68% in a beaker, slowly pouring the sulfuric acid solution with the mass fraction of 70% into concentrated nitric acid along the wall of the beaker, mixing while stirring, then adding the multi-walled carbon nanotubes into the beaker, stirring and reacting for 60min at the rotation speed of 500r/min, filtering to obtain filter residue, washing the filter residue with ammonia water with the mass fraction of 30% until the washing liquid is neutral, then placing the washed filter residue in an oven, and drying to constant weight at the temperature of 110 ℃ to obtain the modified multi-walled carbon nanotubes;
(2) taking 40 parts of graphene oxide, 20 parts of modified fullerene, 2 parts of hydrazine hydrate, 80 parts of water and 30 parts of dimethyl sulfoxide in sequence, placing the graphene oxide and the water into a No. 1 single-neck flask, then placing a three-neck flask into an ultrasonic disperser, mixing ultrasonic waves for 60min under the condition that the ultrasonic frequency is 75kHz to obtain No. 1 dispersion liquid, placing the modified fullerene and the dimethyl sulfoxide into a No. 2 single-neck flask, then placing the three-neck flask into the ultrasonic disperser, mixing ultrasonic waves for 60min under the condition that the ultrasonic frequency is 75kHz to obtain No. 2 dispersion liquid, placing the No. 1 dispersion liquid and the No. 2 dispersion liquid into a hydrothermal reaction kettle, stirring and mixing for 30min under the condition that the rotating speed is 500r/min, then adding the hydrazine hydrate into the hydrothermal reaction kettle, heating and reacting for 8h under the condition that the temperature is 98 ℃, cooling and centrifuging to obtain mixed liquid, then filtering the mixed liquid, obtaining a filter cake, washing the filter cake for 8 times by using absolute ethyl alcohol, and then placing the filter cake in an oven to be dried for 60min to obtain pretreated graphene oxide;
(3) according to the weight parts, 30 parts of pretreated graphene oxide, 30 parts of absolute ethyl alcohol, 5 parts of molybdenum disulfide, 30 parts of nano titanium powder and 20 parts of nano silver powder are taken in sequence, the pretreated graphene oxide, the absolute ethyl alcohol, the nano titanium powder and the nano silver powder are mixed and placed in a ball mill, heating and ball milling is carried out for 60min at the temperature of 220 ℃ to obtain ball grinding materials, then the ball grinding materials are placed in an alloy furnace, chlorine gas is filled into the alloy furnace at the rate of 90mL/min, the mixture is subjected to pressurization and constant temperature reaction for 50min at the pressure of 15MPa and the temperature of 220 ℃, the mixture is heated to 420 ℃, is subjected to constant temperature treatment for 2h, is exhausted, is heated to 1200 ℃ at the rate of 15 ℃/min, is added with molybdenum disulfide, is subjected to nitrogen gas filling into the alloy furnace at the rate of 90mL/min, is stirred and reacts for 8h at the temperature of 1200 ℃, is cooled to 350 ℃, adding rare earth into an alloy furnace, stirring at a constant temperature of 350 ℃ for reaction for 3h, exhausting, adding sodium thiosulfate, cooling and stirring to room temperature, discharging to obtain a treated material, placing the treated material in an oven, and drying at a temperature of 110 ℃ for 60min to obtain modified graphene oxide;
(4) taking 20 parts of furfurylamine, 10 parts of terephthalaldehyde and 30 parts of cardanol in sequence by weight, placing the furfurylamine, the terephthalaldehyde and the cardanol in a four-neck flask, then placing the four-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 60min at a constant temperature of 70 ℃ and at a rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry in a rotary evaporator, and performing rotary evaporation and concentration for 60min at a temperature of 65 ℃ to obtain modified resin;
(5) taking 10 parts of modified multi-walled carbon nanotubes, 20 parts of modified graphene oxide, 20 parts of modified resin, 20 parts of polyol, 2 parts of calcium nitrate and 10 parts of phospholipid in sequence, placing the modified multi-walled carbon nanotubes and the modified graphene oxide in a ball mill, mixing and ball-milling for 60min, adding the modified resin, the calcium nitrate, the polyol and the phospholipid, and ball-milling and mixing for 60min to obtain the alkene alloy lubricating oil additive;
(6) and (6) detecting.
The preparation steps of the modified fullerene in the step (2) are as follows:
(1) taking 2 parts of fullerene C in sequence by weight60200 parts of ethylenediamine, 200 parts of acetone and 30 parts of distilled water, and mixing the fullerene C60Putting ethylenediamine and the mixture into a reactor, introducing nitrogen into the reactor at a rate of 90mL/min, reacting for 60min at a temperature of 82 ℃ and a rotation speed of 800r/min to obtain mixed slurry, putting the mixed slurry into a rotary evaporator, carrying out reduced pressure rotary evaporation for 60min at a temperature of 70 ℃ to obtain concentrated solution, mixing the concentrated solution with distilled water, adding acetone, diluting and crystallizing for 18-24 h, and filtering to obtain pretreated fullerene;
(2) sequentially taking 2 parts of pretreated fullerene, 30 parts of water and 8 parts of 65% nitric acid by weight, placing the pretreated fullerene and the water in a No. 3 single-neck flask, stirring and mixing for 60min at the rotation speed of 600r/min, then adding the nitric acid, then placing the No. 3 single-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 2h at the temperature of 30 ℃ and the rotation speed of 800r/min to obtain a mixed treatment liquid, then placing the mixed treatment liquid in a rotary evaporator, carrying out reduced pressure rotary evaporation for 60min at the temperature of 80 ℃ to obtain concentrated slurry, then placing the concentrated slurry in a vacuum drier, and drying to constant weight to obtain the modified fullerene.
Example 2
The alkene alloy lubricating oil additive comprises the following raw materials in parts by weight: 10 parts of modified multi-walled carbon nanotubes, 20 parts of graphene oxide, 20 parts of modified resin, 20 parts of polyol, 2 parts of calcium nitrate and 10 parts of phospholipid.
The polyhydric alcohol is diethylene glycol.
The phospholipid is soybean phospholipid.
The processing technology of the alkene alloy lubricating oil additive comprises the following processing steps:
(1) according to the weight parts, sequentially taking 5 parts of multi-walled carbon nanotubes, 60 parts of sulfuric acid solution and 10 parts of nitric acid solution, placing the nitric acid solution with the mass fraction of 68% in a beaker, slowly pouring the sulfuric acid solution with the mass fraction of 70% into concentrated nitric acid along the wall of the beaker, mixing while stirring, then adding the multi-walled carbon nanotubes into the beaker, stirring and reacting for 60min at the rotation speed of 500r/min, filtering to obtain filter residue, washing the filter residue with ammonia water with the mass fraction of 30% until the washing liquid is neutral, then placing the washed filter residue in an oven, and drying to constant weight at the temperature of 110 ℃ to obtain the modified multi-walled carbon nanotubes;
(2) taking 20 parts of furfurylamine, 10 parts of terephthalaldehyde and 30 parts of cardanol in sequence by weight, placing the furfurylamine, the terephthalaldehyde and the cardanol in a four-neck flask, then placing the four-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 60min at a constant temperature of 70 ℃ and at a rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry in a rotary evaporator, and performing rotary evaporation and concentration for 60min at a temperature of 65 ℃ to obtain modified resin;
(3) taking 10 parts of modified multi-walled carbon nanotubes, 20 parts of graphene oxide, 20 parts of modified resin, 20 parts of polyol, 2 parts of calcium nitrate and 10 parts of phospholipid in sequence, placing the modified multi-walled carbon nanotubes and the graphene oxide in a ball mill, mixing and ball-milling for 60min, adding the modified resin, the calcium nitrate, the polyol and the phospholipid, and ball-milling and mixing for 60min to obtain the alkene alloy lubricating oil additive;
(4) and (6) detecting.
Example 3
The alkene alloy lubricating oil additive comprises the following raw materials in parts by weight: 10 parts of modified multi-walled carbon nanotube, 20 parts of modified graphene oxide, 20 parts of polyol, 2 parts of calcium nitrate and 10 parts of phospholipid.
The polyhydric alcohol is diethylene glycol.
The phospholipid is soybean phospholipid.
The processing technology of the alkene alloy lubricating oil additive comprises the following processing steps:
(1) according to the weight parts, sequentially taking 5 parts of multi-walled carbon nanotubes, 60 parts of sulfuric acid solution and 10 parts of nitric acid solution, placing the nitric acid solution with the mass fraction of 68% in a beaker, slowly pouring the sulfuric acid solution with the mass fraction of 70% into concentrated nitric acid along the wall of the beaker, mixing while stirring, then adding the multi-walled carbon nanotubes into the beaker, stirring and reacting for 60min at the rotation speed of 500r/min, filtering to obtain filter residue, washing the filter residue with ammonia water with the mass fraction of 30% until the washing liquid is neutral, then placing the washed filter residue in an oven, and drying to constant weight at the temperature of 110 ℃ to obtain the modified multi-walled carbon nanotubes;
(2) taking 40 parts of graphene oxide, 20 parts of modified fullerene, 2 parts of hydrazine hydrate, 80 parts of water and 30 parts of dimethyl sulfoxide in sequence, placing the graphene oxide and the water into a No. 1 single-neck flask, then placing a three-neck flask into an ultrasonic disperser, mixing ultrasonic waves for 60min under the condition that the ultrasonic frequency is 75kHz to obtain No. 1 dispersion liquid, placing the modified fullerene and the dimethyl sulfoxide into a No. 2 single-neck flask, then placing the three-neck flask into the ultrasonic disperser, mixing ultrasonic waves for 60min under the condition that the ultrasonic frequency is 75kHz to obtain No. 2 dispersion liquid, placing the No. 1 dispersion liquid and the No. 2 dispersion liquid into a hydrothermal reaction kettle, stirring and mixing for 30min under the condition that the rotating speed is 500r/min, then adding the hydrazine hydrate into the hydrothermal reaction kettle, heating and reacting for 8h under the condition that the temperature is 98 ℃, cooling and centrifuging to obtain mixed liquid, then filtering the mixed liquid, obtaining a filter cake, washing the filter cake for 8 times by using absolute ethyl alcohol, and then placing the filter cake in an oven to be dried for 60min to obtain pretreated graphene oxide;
(3) according to the weight parts, 30 parts of pretreated graphene oxide, 30 parts of absolute ethyl alcohol, 5 parts of molybdenum disulfide, 30 parts of nano titanium powder and 20 parts of nano silver powder are taken in sequence, the pretreated graphene oxide, the absolute ethyl alcohol, the nano titanium powder and the nano silver powder are mixed and placed in a ball mill, heating and ball milling is carried out for 60min at the temperature of 220 ℃ to obtain ball grinding materials, then the ball grinding materials are placed in an alloy furnace, chlorine gas is filled into the alloy furnace at the rate of 90mL/min, the mixture is subjected to pressurization and constant temperature reaction for 50min at the pressure of 15MPa and the temperature of 220 ℃, the mixture is heated to 420 ℃, is subjected to constant temperature treatment for 2h, is exhausted, is heated to 1200 ℃ at the rate of 15 ℃/min, is added with molybdenum disulfide, is subjected to nitrogen gas filling into the alloy furnace at the rate of 90mL/min, is stirred and reacts for 8h at the temperature of 1200 ℃, is cooled to 350 ℃, adding rare earth into an alloy furnace, stirring at a constant temperature of 350 ℃ for reaction for 3h, exhausting, adding sodium thiosulfate, cooling and stirring to room temperature, discharging to obtain a treated material, placing the treated material in an oven, and drying at a temperature of 110 ℃ for 60min to obtain modified graphene oxide;
(4) taking 10 parts of modified multi-walled carbon nanotubes, 20 parts of modified graphene oxide, 20 parts of polyol, 2 parts of calcium nitrate and 10 parts of phospholipid in sequence, placing the modified multi-walled carbon nanotubes and the modified graphene oxide in a ball mill, mixing and ball-milling for 60min, adding the calcium nitrate, the polyol and the phospholipid, and ball-milling and mixing for 60min to obtain the olefin alloy lubricating oil additive;
(5) and (6) detecting.
The preparation steps of the modified fullerene in the step (2) are as follows:
(1) taking 2 parts of fullerene C in sequence by weight60200 parts of ethylenediamine, 200 parts of acetone and 30 parts of distilled water, and mixing the fullerene C60Putting ethylenediamine and the mixture into a reactor, introducing nitrogen into the reactor at a rate of 90mL/min, reacting for 60min at a temperature of 82 ℃ and a rotation speed of 800r/min to obtain mixed slurry, putting the mixed slurry into a rotary evaporator, carrying out reduced pressure rotary evaporation for 60min at a temperature of 70 ℃ to obtain concentrated solution, mixing the concentrated solution with distilled water, adding acetone, diluting and crystallizing for 18-24 h, and filtering to obtain pretreated fullerene;
(2) sequentially taking 2 parts of pretreated fullerene, 30 parts of water and 8 parts of 65% nitric acid by weight, placing the pretreated fullerene and the water in a No. 3 single-neck flask, stirring and mixing for 60min at the rotation speed of 600r/min, then adding the nitric acid, then placing the No. 3 single-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 2h at the temperature of 30 ℃ and the rotation speed of 800r/min to obtain a mixed treatment liquid, then placing the mixed treatment liquid in a rotary evaporator, carrying out reduced pressure rotary evaporation for 60min at the temperature of 80 ℃ to obtain concentrated slurry, then placing the concentrated slurry in a vacuum drier, and drying to constant weight to obtain the modified fullerene.
Example 4
The alkene alloy lubricating oil additive comprises the following raw materials in parts by weight: 10 parts of modified multi-walled carbon nanotubes, 20 parts of modified graphene oxide, 20 parts of modified resin, 20 parts of polyol and 10 parts of phospholipid.
The polyhydric alcohol is diethylene glycol.
The phospholipid is soybean phospholipid.
The processing technology of the alkene alloy lubricating oil additive comprises the following processing steps:
(1) according to the weight parts, sequentially taking 5 parts of multi-walled carbon nanotubes, 60 parts of sulfuric acid solution and 10 parts of nitric acid solution, placing the nitric acid solution with the mass fraction of 68% in a beaker, slowly pouring the sulfuric acid solution with the mass fraction of 70% into concentrated nitric acid along the wall of the beaker, mixing while stirring, then adding the multi-walled carbon nanotubes into the beaker, stirring and reacting for 60min at the rotation speed of 500r/min, filtering to obtain filter residue, washing the filter residue with ammonia water with the mass fraction of 30% until the washing liquid is neutral, then placing the washed filter residue in an oven, and drying to constant weight at the temperature of 110 ℃ to obtain the modified multi-walled carbon nanotubes;
(2) taking 40 parts of graphene oxide, 20 parts of modified fullerene, 2 parts of hydrazine hydrate, 80 parts of water and 30 parts of dimethyl sulfoxide in sequence, placing the graphene oxide and the water into a No. 1 single-neck flask, then placing a three-neck flask into an ultrasonic disperser, mixing ultrasonic waves for 60min under the condition that the ultrasonic frequency is 75kHz to obtain No. 1 dispersion liquid, placing the modified fullerene and the dimethyl sulfoxide into a No. 2 single-neck flask, then placing the three-neck flask into the ultrasonic disperser, mixing ultrasonic waves for 60min under the condition that the ultrasonic frequency is 75kHz to obtain No. 2 dispersion liquid, placing the No. 1 dispersion liquid and the No. 2 dispersion liquid into a hydrothermal reaction kettle, stirring and mixing for 30min under the condition that the rotating speed is 500r/min, then adding the hydrazine hydrate into the hydrothermal reaction kettle, heating and reacting for 8h under the condition that the temperature is 98 ℃, cooling and centrifuging to obtain mixed liquid, then filtering the mixed liquid, obtaining a filter cake, washing the filter cake for 8 times by using absolute ethyl alcohol, and then placing the filter cake in an oven to be dried for 60min to obtain pretreated graphene oxide;
(3) according to the weight parts, 30 parts of pretreated graphene oxide, 30 parts of absolute ethyl alcohol, 5 parts of molybdenum disulfide, 30 parts of nano titanium powder and 20 parts of nano silver powder are taken in sequence, the pretreated graphene oxide, the absolute ethyl alcohol, the nano titanium powder and the nano silver powder are mixed and placed in a ball mill, heating and ball milling is carried out for 60min at the temperature of 220 ℃ to obtain ball grinding materials, then the ball grinding materials are placed in an alloy furnace, chlorine gas is filled into the alloy furnace at the rate of 90mL/min, the mixture is subjected to pressurization and constant temperature reaction for 50min at the pressure of 15MPa and the temperature of 220 ℃, the mixture is heated to 420 ℃, is subjected to constant temperature treatment for 2h, is exhausted, is heated to 1200 ℃ at the rate of 15 ℃/min, is added with molybdenum disulfide, is subjected to nitrogen gas filling into the alloy furnace at the rate of 90mL/min, is stirred and reacts for 8h at the temperature of 1200 ℃, is cooled to 350 ℃, adding rare earth into an alloy furnace, stirring at a constant temperature of 350 ℃ for reaction for 3h, exhausting, adding sodium thiosulfate, cooling and stirring to room temperature, discharging to obtain a treated material, placing the treated material in an oven, and drying at a temperature of 110 ℃ for 60min to obtain modified graphene oxide;
(4) taking 20 parts of furfurylamine, 10 parts of terephthalaldehyde and 30 parts of cardanol in sequence by weight, placing the furfurylamine, the terephthalaldehyde and the cardanol in a four-neck flask, then placing the four-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 60min at a constant temperature of 70 ℃ and at a rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry in a rotary evaporator, and performing rotary evaporation and concentration for 60min at a temperature of 65 ℃ to obtain modified resin;
(5) taking 10 parts of modified multi-walled carbon nanotubes, 20 parts of modified graphene oxide, 20 parts of modified resin, 20 parts of polyol and 10 parts of phospholipid in sequence, placing the modified multi-walled carbon nanotubes and the modified graphene oxide in a ball mill, mixing and ball-milling for 60min, adding the modified resin, the polyol and the phospholipid, and ball-milling and mixing for 60min to obtain the olefin alloy lubricating oil additive;
(6) and (6) detecting.
The preparation steps of the modified fullerene in the step (2) are as follows:
(1) taking 2 parts of fullerene C in sequence by weight60200 parts of ethylenediamine, 200 parts of acetone and 30 parts of distilled water, and mixing the fullerene C60Putting ethylenediamine and the mixture into a reactor, introducing nitrogen into the reactor at a rate of 90mL/min, reacting for 60min at a temperature of 82 ℃ and a rotation speed of 800r/min to obtain mixed slurry, putting the mixed slurry into a rotary evaporator, carrying out reduced pressure rotary evaporation for 60min at a temperature of 70 ℃ to obtain concentrated solution, mixing the concentrated solution with distilled water, adding acetone, diluting and crystallizing for 18-24 h, and filtering to obtain pretreated fullerene;
(2) sequentially taking 2 parts of pretreated fullerene, 30 parts of water and 8 parts of 65% nitric acid by weight, placing the pretreated fullerene and the water in a No. 3 single-neck flask, stirring and mixing for 60min at the rotation speed of 600r/min, then adding the nitric acid, then placing the No. 3 single-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 2h at the temperature of 30 ℃ and the rotation speed of 800r/min to obtain a mixed treatment liquid, then placing the mixed treatment liquid in a rotary evaporator, carrying out reduced pressure rotary evaporation for 60min at the temperature of 80 ℃ to obtain concentrated slurry, then placing the concentrated slurry in a vacuum drier, and drying to constant weight to obtain the modified fullerene.
Example 5
The alkene alloy lubricating oil additive comprises the following raw materials in parts by weight: 10 parts of multi-walled carbon nanotube, 20 parts of modified graphene oxide, 20 parts of modified resin, 20 parts of polyol, 2 parts of calcium nitrate and 10 parts of phospholipid.
The polyhydric alcohol is diethylene glycol.
The phospholipid is soybean phospholipid.
The processing technology of the alkene alloy lubricating oil additive comprises the following processing steps:
(1) taking 40 parts of graphene oxide, 20 parts of modified fullerene, 2 parts of hydrazine hydrate, 80 parts of water and 30 parts of dimethyl sulfoxide in sequence, placing the graphene oxide and the water into a No. 1 single-neck flask, then placing a three-neck flask into an ultrasonic disperser, mixing ultrasonic waves for 60min under the condition that the ultrasonic frequency is 75kHz to obtain No. 1 dispersion liquid, placing the modified fullerene and the dimethyl sulfoxide into a No. 2 single-neck flask, then placing the three-neck flask into the ultrasonic disperser, mixing ultrasonic waves for 60min under the condition that the ultrasonic frequency is 75kHz to obtain No. 2 dispersion liquid, placing the No. 1 dispersion liquid and the No. 2 dispersion liquid into a hydrothermal reaction kettle, stirring and mixing for 30min under the condition that the rotating speed is 500r/min, then adding the hydrazine hydrate into the hydrothermal reaction kettle, heating and reacting for 8h under the condition that the temperature is 98 ℃, cooling and centrifuging to obtain mixed liquid, then filtering the mixed liquid, obtaining a filter cake, washing the filter cake for 8 times by using absolute ethyl alcohol, and then placing the filter cake in an oven to be dried for 60min to obtain pretreated graphene oxide;
(2) according to the weight parts, 30 parts of pretreated graphene oxide, 30 parts of absolute ethyl alcohol, 5 parts of molybdenum disulfide, 30 parts of nano titanium powder and 20 parts of nano silver powder are taken in sequence, the pretreated graphene oxide, the absolute ethyl alcohol, the nano titanium powder and the nano silver powder are mixed and placed in a ball mill, heating and ball milling is carried out for 60min at the temperature of 220 ℃ to obtain ball grinding materials, then the ball grinding materials are placed in an alloy furnace, chlorine gas is filled into the alloy furnace at the rate of 90mL/min, the mixture is subjected to pressurization and constant temperature reaction for 50min at the pressure of 15MPa and the temperature of 220 ℃, the mixture is heated to 420 ℃, is subjected to constant temperature treatment for 2h, is exhausted, is heated to 1200 ℃ at the rate of 15 ℃/min, is added with molybdenum disulfide, is subjected to nitrogen gas filling into the alloy furnace at the rate of 90mL/min, is stirred and reacts for 8h at the temperature of 1200 ℃, is cooled to 350 ℃, adding rare earth into an alloy furnace, stirring at a constant temperature of 350 ℃ for reaction for 3h, exhausting, adding sodium thiosulfate, cooling and stirring to room temperature, discharging to obtain a treated material, placing the treated material in an oven, and drying at a temperature of 110 ℃ for 60min to obtain modified graphene oxide;
(3) taking 20 parts of furfurylamine, 10 parts of terephthalaldehyde and 30 parts of cardanol in sequence by weight, placing the furfurylamine, the terephthalaldehyde and the cardanol in a four-neck flask, then placing the four-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 60min at a constant temperature of 70 ℃ and at a rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry in a rotary evaporator, and performing rotary evaporation and concentration for 60min at a temperature of 65 ℃ to obtain modified resin;
(4) sequentially taking 10 parts of multi-walled carbon nanotubes, 20 parts of modified graphene oxide, 20 parts of modified resin, 20 parts of polyol, 2 parts of calcium nitrate and 10 parts of phospholipid, putting the multi-walled carbon nanotubes and the modified graphene oxide into a ball mill, mixing and ball-milling for 60min, adding the modified resin, the calcium nitrate, the polyol and the phospholipid, and ball-milling and mixing for 60min to obtain the olefin alloy lubricating oil additive;
(5) and (6) detecting.
The preparation steps of the modified fullerene in the step (1) are as follows:
(1) taking 2 parts of fullerene C in sequence by weight60200 parts of ethylenediamine, 200 parts of acetone and 30 parts of distilled water, and mixing the fullerene C60And ethylene diamine in the reactionFilling nitrogen into a reactor at a rate of 90mL/min, reacting for 60min at a temperature of 82 ℃ and a rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry into a rotary evaporator, carrying out reduced pressure rotary evaporation for 60min at a temperature of 70 ℃ to obtain concentrated solution, mixing the concentrated solution with distilled water, then adding acetone, diluting and crystallizing for 18-24 h, and filtering to obtain pretreated fullerene;
(2) sequentially taking 2 parts of pretreated fullerene, 30 parts of water and 8 parts of 65% nitric acid by weight, placing the pretreated fullerene and the water in a No. 3 single-neck flask, stirring and mixing for 60min at the rotation speed of 600r/min, then adding the nitric acid, then placing the No. 3 single-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 2h at the temperature of 30 ℃ and the rotation speed of 800r/min to obtain a mixed treatment liquid, then placing the mixed treatment liquid in a rotary evaporator, carrying out reduced pressure rotary evaporation for 60min at the temperature of 80 ℃ to obtain concentrated slurry, then placing the concentrated slurry in a vacuum drier, and drying to constant weight to obtain the modified fullerene.
Example 6
The alkene alloy lubricating oil additive comprises the following raw materials in parts by weight: 10 parts of modified multi-walled carbon nanotube, 20 parts of modified graphene oxide, 20 parts of modified resin, 20 parts of polyol and 2 parts of calcium nitrate.
The polyhydric alcohol is diethylene glycol.
The processing technology of the alkene alloy lubricating oil additive comprises the following processing steps:
(1) according to the weight parts, sequentially taking 5 parts of multi-walled carbon nanotubes, 60 parts of sulfuric acid solution and 10 parts of nitric acid solution, placing the nitric acid solution with the mass fraction of 68% in a beaker, slowly pouring the sulfuric acid solution with the mass fraction of 70% into concentrated nitric acid along the wall of the beaker, mixing while stirring, then adding the multi-walled carbon nanotubes into the beaker, stirring and reacting for 60min at the rotation speed of 500r/min, filtering to obtain filter residue, washing the filter residue with ammonia water with the mass fraction of 30% until the washing liquid is neutral, then placing the washed filter residue in an oven, and drying to constant weight at the temperature of 110 ℃ to obtain the modified multi-walled carbon nanotubes;
(2) taking 40 parts of graphene oxide, 20 parts of modified fullerene, 2 parts of hydrazine hydrate, 80 parts of water and 30 parts of dimethyl sulfoxide in sequence, placing the graphene oxide and the water into a No. 1 single-neck flask, then placing a three-neck flask into an ultrasonic disperser, mixing ultrasonic waves for 60min under the condition that the ultrasonic frequency is 75kHz to obtain No. 1 dispersion liquid, placing the modified fullerene and the dimethyl sulfoxide into a No. 2 single-neck flask, then placing the three-neck flask into the ultrasonic disperser, mixing ultrasonic waves for 60min under the condition that the ultrasonic frequency is 75kHz to obtain No. 2 dispersion liquid, placing the No. 1 dispersion liquid and the No. 2 dispersion liquid into a hydrothermal reaction kettle, stirring and mixing for 30min under the condition that the rotating speed is 500r/min, then adding the hydrazine hydrate into the hydrothermal reaction kettle, heating and reacting for 8h under the condition that the temperature is 98 ℃, cooling and centrifuging to obtain mixed liquid, then filtering the mixed liquid, obtaining a filter cake, washing the filter cake for 8 times by using absolute ethyl alcohol, and then placing the filter cake in an oven to be dried for 60min to obtain pretreated graphene oxide;
(3) according to the weight parts, 30 parts of pretreated graphene oxide, 30 parts of absolute ethyl alcohol, 5 parts of molybdenum disulfide, 30 parts of nano titanium powder and 20 parts of nano silver powder are taken in sequence, the pretreated graphene oxide, the absolute ethyl alcohol, the nano titanium powder and the nano silver powder are mixed and placed in a ball mill, heating and ball milling is carried out for 60min at the temperature of 220 ℃ to obtain ball grinding materials, then the ball grinding materials are placed in an alloy furnace, chlorine gas is filled into the alloy furnace at the rate of 90mL/min, the mixture is subjected to pressurization and constant temperature reaction for 50min at the pressure of 15MPa and the temperature of 220 ℃, the mixture is heated to 420 ℃, is subjected to constant temperature treatment for 2h, is exhausted, is heated to 1200 ℃ at the rate of 15 ℃/min, is added with molybdenum disulfide, is subjected to nitrogen gas filling into the alloy furnace at the rate of 90mL/min, is stirred and reacts for 8h at the temperature of 1200 ℃, is cooled to 350 ℃, adding rare earth into an alloy furnace, stirring at a constant temperature of 350 ℃ for reaction for 3h, exhausting, adding sodium thiosulfate, cooling and stirring to room temperature, discharging to obtain a treated material, placing the treated material in an oven, and drying at a temperature of 110 ℃ for 60min to obtain modified graphene oxide;
(4) taking 20 parts of furfurylamine, 10 parts of terephthalaldehyde and 30 parts of cardanol in sequence by weight, placing the furfurylamine, the terephthalaldehyde and the cardanol in a four-neck flask, then placing the four-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 60min at a constant temperature of 70 ℃ and at a rotating speed of 800r/min to obtain mixed slurry, then placing the mixed slurry in a rotary evaporator, and performing rotary evaporation and concentration for 60min at a temperature of 65 ℃ to obtain modified resin;
(5) taking 10 parts of modified multi-walled carbon nanotubes, 20 parts of modified graphene oxide, 20 parts of modified resin, 20 parts of polyol and 2 parts of calcium nitrate in sequence, placing the modified multi-walled carbon nanotubes and the modified graphene oxide in a ball mill, mixing and ball-milling for 60min, adding the modified resin, the calcium nitrate and the polyol, and ball-milling and mixing for 60min to obtain the olefin alloy lubricating oil additive;
(6) and (6) detecting.
The preparation steps of the modified fullerene in the step (2) are as follows:
(1) taking 2 parts of fullerene C in sequence by weight60200 parts of ethylenediamine, 200 parts of acetone and 30 parts of distilled water, and mixing the fullerene C60Putting ethylenediamine and the mixture into a reactor, introducing nitrogen into the reactor at a rate of 90mL/min, reacting for 60min at a temperature of 82 ℃ and a rotation speed of 800r/min to obtain mixed slurry, putting the mixed slurry into a rotary evaporator, carrying out reduced pressure rotary evaporation for 60min at a temperature of 70 ℃ to obtain concentrated solution, mixing the concentrated solution with distilled water, adding acetone, diluting and crystallizing for 18-24 h, and filtering to obtain pretreated fullerene;
(2) sequentially taking 2 parts of pretreated fullerene, 30 parts of water and 8 parts of 65% nitric acid by weight, placing the pretreated fullerene and the water in a No. 3 single-neck flask, stirring and mixing for 60min at the rotation speed of 600r/min, then adding the nitric acid, then placing the No. 3 single-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 2h at the temperature of 30 ℃ and the rotation speed of 800r/min to obtain a mixed treatment liquid, then placing the mixed treatment liquid in a rotary evaporator, carrying out reduced pressure rotary evaporation for 60min at the temperature of 80 ℃ to obtain concentrated slurry, then placing the concentrated slurry in a vacuum drier, and drying to constant weight to obtain the modified fullerene.
Comparative example
The alkene alloy lubricating oil additive comprises the following raw materials in parts by weight: 10 parts of multi-walled carbon nanotube, 20 parts of graphene oxide, 20 parts of polyol and 2 parts of calcium nitrate.
The polyhydric alcohol is diethylene glycol.
The processing technology of the alkene alloy lubricating oil additive comprises the following processing steps:
(1) sequentially taking 10 parts of multi-walled carbon nanotubes, 20 parts of graphene oxide, 20 parts of polyol and 2 parts of calcium nitrate, putting the multi-walled carbon nanotubes and the graphene oxide into a ball mill, mixing and ball-milling for 60min, then adding the calcium nitrate and the polyol, and ball-milling and mixing for 60min to obtain the olefin alloy lubricating oil additive;
(2) and (6) detecting.
Performance test table: TABLE 1
Figure BDA0002232643870000261
As can be seen from table 1: compared with the comparative example, the modified graphene oxide is added, the ultrathin lamellar structure of the graphene oxide is easy to enter a contact surface, the direct contact of rough surfaces is reduced, the modified fullerene can inhibit the agglomeration of the graphene oxide due to the hollow spherical structure of the fullerene, the sliding action of the two contact surfaces can be increased by attaching the modified fullerene between the graphene oxide lamellar layers, a lubricating film is formed on the friction surface, the antifriction performance of lubricating oil is improved, the spherical fullerene ball structure has good elasticity, the contact of the friction surface can be effectively blocked, and the abrasion resistance of a product is further improved; by comparing examples 1, 4 and 6 with comparative examples, after the multi-walled carbon nanotube is subjected to mixed acid treatment, the surface of the multi-walled carbon nanotube contains a large number of oxygen-containing groups, and in the using process, the modified multi-walled carbon nanotube can be combined with hydrophilic groups on the surface of modified graphene oxide, so that the oil solubility of the modified graphene oxide can be effectively improved, the graphene oxide can be well dispersed in a system, and the wear resistance of a product can be further improved; by comparing the examples 1 and 5 with the comparative examples, in the using process, the phospholipid can be decomposed by high temperature in the system, the decomposed polyphosphoric acid can be combined with calcium ions in the system to form calcium hydroxy phosphate, and the obtained calcium hydroxy phosphate is attached to the damage of the friction surface, so that the damage of the friction surface can be effectively repaired, and the wear resistance of the product is further improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (10)

1. An olefin alloy lubricating oil additive is characterized in that: the composite material comprises the following raw materials in parts by weight: 8-10 parts of modified multi-walled carbon nanotubes, 10-20 parts of modified graphene oxide, 10-20 parts of modified resin, 10-20 parts of polyhydric alcohol, 1-2 parts of calcium nitrate and 8-10 parts of phospholipid.
2. The olefinic alloy lubricating oil additive as claimed in claim 1, wherein: the polyhydric alcohol is any one of diethylene glycol, dipropylene glycol or trimethylolpropane; the phospholipid is any one of soybean phospholipid, yolk phospholipid or peanut phospholipid.
3. The olefinic alloy lubricating oil additive as claimed in claim 1, wherein: the modified multi-walled carbon nanotube is prepared by modifying a multi-walled carbon nanotube, a sulfuric acid solution and a nitric acid solution.
4. The olefinic alloy lubricating oil additive as claimed in claim 1, wherein: the modified graphene oxide is prepared by modifying pretreated graphene oxide, absolute ethyl alcohol, molybdenum disulfide, nano titanium powder and nano silver powder; the pretreated graphene oxide is prepared by modifying graphene oxide, modified fullerene, hydrazine hydrate, water and dimethyl sulfoxide.
5. The olefinic alloy lubricating oil additive as claimed in claim 1, wherein: the modified resin is prepared by modifying furfuryl amine, terephthalaldehyde and cardanol.
6. The olefinic alloy lubricating oil additive as claimed in claim 1, wherein: the alkene alloy lubricating oil additive comprises the following raw materials in parts by weight: 10 parts of modified multi-walled carbon nanotube, 20 parts of modified graphene oxide, 20 parts of modified resin, 20 parts of polyol, 2 parts of calcium nitrate and 10 parts of phospholipid.
7. The processing technology of the alkene alloy lubricating oil additive is characterized by comprising the following specific preparation steps:
(1) processing the multi-walled carbon nanotubes;
(2) pretreating graphene oxide;
(3) modifying the product obtained in the step (2);
(4) preparing modified resin;
(5) mixing materials;
(6) and (6) detecting.
8. The process of claim 7, wherein the olefin alloy lubricating oil additive is prepared by the following steps: the processing steps of the alkene alloy lubricating oil additive are as follows:
(1) mixing a sulfuric acid solution and a nitric acid solution, then adding the multi-walled carbon nano tube, stirring for reaction, filtering, washing and drying to obtain a modified multi-walled carbon nano tube;
(2) mixing graphene oxide with water and performing ultrasonic treatment to obtain No. 1 dispersion liquid, mixing modified fullerene with dimethyl sulfoxide and performing ultrasonic treatment to obtain No. 2 dispersion liquid, stirring and mixing the No. 1 dispersion liquid and the No. 2 dispersion liquid, adding hydrazine hydrate, performing heating reaction, cooling and centrifuging, filtering, washing and drying to obtain pretreated graphene oxide;
(3) mixing the pretreated graphene oxide, absolute ethyl alcohol, nano titanium powder and nano silver powder, heating, ball milling, filling chlorine, pressurizing, reacting at constant temperature, heating, exhausting, heating step by step, adding molybdenum disulfide, filling nitrogen for reacting, cooling, adding rare earth, stirring at constant temperature for reacting, exhausting, adding sodium thiosulfate, cooling, stirring to room temperature, and drying to obtain modified graphene oxide;
(4) mixing furfuryl amine, terephthalaldehyde and cardanol, stirring at constant temperature for reaction, and performing rotary evaporation and concentration to obtain modified resin;
(5) mixing and ball-milling the modified multi-walled carbon nanotubes and the modified graphene oxide, then adding the modified resin, calcium nitrate, polyol and phospholipid, and ball-milling and mixing to obtain the olefin alloy lubricating oil additive;
(6) and (6) detecting.
9. The process of claim 8, wherein the olefin alloy lubricating oil additive is prepared by the following steps: the processing process of the alkene alloy lubricating oil additive is as follows:
(1) putting a nitric acid solution with the mass fraction of 68% into a beaker, slowly pouring a sulfuric acid solution with the mass fraction of 70% into concentrated nitric acid along the wall of the beaker, mixing while stirring, adding a multi-walled carbon nanotube into the beaker, stirring and reacting for 40-60 min at the rotation speed of 400-500 r/min, filtering to obtain filter residue, washing the filter residue with ammonia water with the mass fraction of 20-30% until the washing liquid is neutral, then putting the washed filter residue into an oven, and drying at the temperature of 105-110 ℃ to constant weight to obtain the modified multi-walled carbon nanotube;
(2) placing graphene oxide and water into a No. 1 single-neck flask, placing a three-neck flask into an ultrasonic disperser, mixing ultrasonic waves for 40-60 min under the condition that the ultrasonic frequency is 55-75 kHz to obtain No. 1 dispersion liquid, placing modified fullerene and dimethyl sulfoxide into a No. 2 single-neck flask, placing the three-neck flask into the ultrasonic disperser, mixing ultrasonic waves for 40-60 min under the condition that the ultrasonic frequency is 55-75 kHz to obtain No. 2 dispersion liquid, placing the No. 1 dispersion liquid and the No. 2 dispersion liquid into a hydrothermal reaction kettle, stirring and mixing for 10-30 min under the condition that the rotating speed is 300-500 r/min, adding hydrazine hydrate into the hydrothermal reaction kettle, heating and reacting for 6-8 h under the condition that the temperature is 96-98 ℃, cooling and centrifuging to obtain mixed liquid, filtering the mixed liquid to obtain filter cakes, washing the filter cakes for 5-8 times by using absolute ethyl alcohol, then, placing the filter cake in an oven, and drying for 40-60 min to obtain pretreated graphene oxide;
(3) mixing pretreated graphene oxide, absolute ethyl alcohol, nano titanium powder and nano silver powder, placing the mixture in a ball mill, heating and ball milling for 40-60 min at the temperature of 200-220 ℃ to obtain a ball grinding material, then placing the ball grinding material in an alloy furnace, filling chlorine gas into the alloy furnace at the speed of 60-90 mL/min, pressurizing and reacting at the pressure of 12-15 MPa and the temperature of 200-220 ℃ for 30-50 min, heating to the temperature of 420 ℃, carrying out constant temperature treatment for 1-2 h, exhausting, heating to the temperature of 1100-1200 ℃ at the speed of 10-15 ℃/min, then adding molybdenum disulfide into the alloy furnace, filling nitrogen gas into the alloy furnace at the speed of 60-90 mL/min, stirring and reacting at the temperature of 1100-1200 ℃ for 5-8 h, cooling to 320-350 ℃, then adding rare earth into the alloy furnace, adding rare earth into the alloy furnace at the temperature of 320-350 ℃, stirring at constant temperature for reaction for 2-3 h, exhausting, adding sodium thiosulfate, cooling and stirring to room temperature, discharging to obtain a treated material, placing the treated material in an oven, and drying at 105-110 ℃ for 40-60 min to obtain modified graphene oxide;
(4) placing furfuryl amine, terephthalaldehyde and cardanol into a four-neck flask, then placing the four-neck flask into a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 40-60 min at a constant temperature under the conditions that the temperature is 65-70 ℃ and the rotating speed is 500-800 r/min to obtain mixed slurry, then placing the mixed slurry into a rotary evaporator, and performing rotary evaporation and concentration for 40-60 min under the conditions that the temperature is 60-65 ℃ to obtain modified resin;
(5) placing the modified multi-walled carbon nanotube and the modified graphene oxide in a ball mill, mixing and ball-milling for 40-60 min, adding modified resin, calcium nitrate, polyol and phospholipid, and ball-milling and mixing for 40-60 min to obtain the alkene alloy lubricating oil additive;
(6) and (6) detecting.
10. The process of claim 9 for processing an olefin alloy lubricating oil additive, wherein: the preparation steps of the modified fullerene in the step (2) are as follows:
(1) sequentially taking 1-2 parts of fullerene C by weight60100-200 parts of ethylenediamine, 100-200 parts of acetone, 20-30 parts of distilled water, and mixing the fullerene C60Putting ethylenediamine and the mixture into a reactor, introducing nitrogen into the reactor at a rate of 60-90 mL/min, reacting for 40-60 min at a temperature of 80-82 ℃ and a rotation speed of 600-800 r/min to obtain mixed slurry, putting the mixed slurry into a rotary evaporator, carrying out reduced pressure rotary evaporation for 40-60 min at a temperature of 60-70 ℃ to obtain concentrated solution, mixing the concentrated solution with distilled water, adding acetone, diluting and crystallizing for 18-24 h, and filtering to obtain pretreated fullerene;
(2) taking 1-2 parts by weight of pretreated fullerene, 20-30 parts by weight of water and 5-8 parts by weight of 65% nitric acid in sequence, placing the pretreated fullerene and the water in a No. 3 single-neck flask, stirring and mixing for 40-60 min at the rotating speed of 400-600 r/min, adding the nitric acid, placing the No. 3 single-neck flask in a digital display speed measurement constant-temperature magnetic stirrer, stirring and reacting for 1-2 h at the temperature of 26-30 ℃ and the rotating speed of 600-800 r/min to obtain a mixed treatment liquid, placing the mixed treatment liquid in a rotary evaporator, decompressing and carrying out rotary evaporation for 40-60 min at the temperature of 70-80 ℃ to obtain concentrated slurry, placing the concentrated slurry in a vacuum drier, and drying to constant weight to obtain the modified fullerene.
CN201910972775.8A 2019-10-14 2019-10-14 Alkene alloy lubricating oil additive and processing technology thereof Pending CN110819423A (en)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7871533B1 (en) * 2006-01-12 2011-01-18 South Dakota School Of Mines And Technology Carbon nanoparticle-containing nanofluid
CN102585973A (en) * 2012-02-08 2012-07-18 哈尔滨工业大学 Preparation method of graphene oxide-fullerene water-based lubricating additives
US20150147012A1 (en) * 2013-11-27 2015-05-28 Emerson Climate Technologies, Inc. Bearing performance for compressors using high energy refrigerants with sulfur-based oil additives
CN106367192A (en) * 2016-08-30 2017-02-01 天长市润达金属防锈助剂有限公司 Lubricating type microemulsion cutting fluid and preparation method thereof
CN106566611A (en) * 2016-10-21 2017-04-19 马鞍山天宇船舶制造有限公司 Weathering-resistant molybdenum disulfide dry film lubricant for self-hold nuts, and production method thereof
CN106675738A (en) * 2016-12-11 2017-05-17 唐林元 Preparation method of metal drawing lubricant
CN107033994A (en) * 2017-05-03 2017-08-11 杭州高烯科技有限公司 A kind of Ba-grease containing spitball shape graphene microballoon and preparation method thereof
US20180022652A1 (en) * 2012-03-02 2018-01-25 Dynamic Material Systems, LLC Composite Ceramics and Ceramic Particles and Method for Producing Ceramic Particles and Bulk Ceramic Particles
CN109181822A (en) * 2018-08-29 2019-01-11 佛山朝鸿新材料科技有限公司 A kind of Hmp grease
CN109912650A (en) * 2019-04-16 2019-06-21 中国科学院宁波材料技术与工程研究所 A kind of phosphorus-nitrogen system biology based flameproofing and its synthetic method and application

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7871533B1 (en) * 2006-01-12 2011-01-18 South Dakota School Of Mines And Technology Carbon nanoparticle-containing nanofluid
CN102585973A (en) * 2012-02-08 2012-07-18 哈尔滨工业大学 Preparation method of graphene oxide-fullerene water-based lubricating additives
US20180022652A1 (en) * 2012-03-02 2018-01-25 Dynamic Material Systems, LLC Composite Ceramics and Ceramic Particles and Method for Producing Ceramic Particles and Bulk Ceramic Particles
US20150147012A1 (en) * 2013-11-27 2015-05-28 Emerson Climate Technologies, Inc. Bearing performance for compressors using high energy refrigerants with sulfur-based oil additives
CN105765246A (en) * 2013-11-27 2016-07-13 艾默生环境优化技术有限公司 Bearing performance for compressors using high energy refrigerants with sulfur-based oil additives
CN106367192A (en) * 2016-08-30 2017-02-01 天长市润达金属防锈助剂有限公司 Lubricating type microemulsion cutting fluid and preparation method thereof
CN106566611A (en) * 2016-10-21 2017-04-19 马鞍山天宇船舶制造有限公司 Weathering-resistant molybdenum disulfide dry film lubricant for self-hold nuts, and production method thereof
CN106675738A (en) * 2016-12-11 2017-05-17 唐林元 Preparation method of metal drawing lubricant
CN107033994A (en) * 2017-05-03 2017-08-11 杭州高烯科技有限公司 A kind of Ba-grease containing spitball shape graphene microballoon and preparation method thereof
CN109181822A (en) * 2018-08-29 2019-01-11 佛山朝鸿新材料科技有限公司 A kind of Hmp grease
CN109912650A (en) * 2019-04-16 2019-06-21 中国科学院宁波材料技术与工程研究所 A kind of phosphorus-nitrogen system biology based flameproofing and its synthetic method and application

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